CN108867165A - A kind of preparation method of silk gum paper sizing agent - Google Patents

A kind of preparation method of silk gum paper sizing agent Download PDF

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Publication number
CN108867165A
CN108867165A CN201810811276.6A CN201810811276A CN108867165A CN 108867165 A CN108867165 A CN 108867165A CN 201810811276 A CN201810811276 A CN 201810811276A CN 108867165 A CN108867165 A CN 108867165A
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silk gum
sizing agent
chitosan
solution
aqueous solution
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CN201810811276.6A
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Chinese (zh)
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王晚秀
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    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00Coated paper; Coating material
    • D21H19/10Coatings without pigments
    • D21H19/14Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • D21H21/16Sizing or water-repelling agents

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  • Paper (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The present invention provides a kind of preparation methods of silk gum paper sizing agent, include the following steps:S1. reeling mill is discarded into degumming liquid filtering, solution is placed in water-bath, is concentrated in vacuo;S2. concentrate is put into bag filter, and dialysis is removed to metal ion, obtains silk gum aqueous solution, silk gum then is obtained by filtration in silk gum aqueous solution;S3. dehydrated alcohol in the silk gum prepared by step S2 filters crystallization, obtains silk gum crystallization;S4. silk gum is slowly dissolve into water, configures silk gum aqueous solution;S5. by chitosan stirring and dissolving in acetic acid solution;S6. silk gum aqueous solution is mixed with chitosan solution, and 1,2,3,4- butane tetracarboxylic acid is added, sodium lauryl sulfate, catalyst, phytosterol, oxidizing glucose aldehyde, obtained silk gum and chitosan blending surface sizing agent, stirring heat preservation are spare.The present invention makes full use of waste resource, prepares a kind of paper surface sizing agent haveing excellent performance.

Description

A kind of preparation method of silk gum paper sizing agent
Technical field
The present invention relates to composite paper sizing agents, and in particular to a kind of preparation method of silk gum paper sizing agent.
Background technique
Silk gum is normally used as waste and discharges with waste water in silk process.China is silk big country, several Over thousand, silk is only used to always filature knit silk fabric, production clothes, and silk gum is not utilized always.Annual production raw silk About 60,000-8 ten thousand tons, the several hundred million rice of silk broadcloth, meet people clothing need while, have 30,000 tons or so of sericine with It produces waste water to be lost, the content of organics such as silk gum in silk production waste water is caused to severely exceed, a large amount of dissolved oxygens consumed in water, Make water eutrophication, lose self-purification capacity, not only pollute environment, but also wastes precious sericine resource.Shell is poly- Sugar is the natural high molecular substance that content is only second to cellulose in nature, resourceful, nontoxic, tasteless, antithrombotic, resist it is quiet Electric, alkaline-resisting, film forming and biocompatibility are good.Chitosan class Cypres are improving wood as a kind of biopolymer Apparent advantage is all shown in terms of the intensity and printing performance of material fibre paper.This research is poly- based on natural organic matter shell Sugar, silk gum and the excellent film forming of the two are mixed applied to top sizing with silk gum using degradation chitosan, reach silk waste water Effective recycling of middle sericine, brings great economic benefit to silk industry.
Summary of the invention
Technical problems to be solved:The object of the present invention is to provide a kind of silk gum paper sizing agent, make full use of discarded money Source prepares a kind of paper surface sizing agent haveing excellent performance.
Technical solution:A kind of preparation method of silk gum paper sizing agent, includes the following steps:
S1. reeling mill is discarded into degumming liquid filtering, solution is placed in 60-70 DEG C of water-bath, is concentrated in vacuo;
S2. concentrate is put into bag filter, and dialysis is removed to metal ion, obtains silk gum aqueous solution, then that silk gum is water-soluble Silk gum is obtained by filtration in liquid;
S3. the dehydrated alcohol of 3-6 times of parts by weight is added in the silk gum prepared by step S2, filters 12h at 4 DEG C, must crystallize, It is washed with ethyl alcohol and is filtered again twice again, it is dry under the conditions of 60-70 DEG C, obtain silk gum crystallization;
S4. silk gum is slowly dissolve into water, configures silk gum aqueous solution, the mass fraction for obtaining silk gum aqueous solution is 4-8%;
S5. by chitosan stirring and dissolving in 0.2 mol/L acetic acid solution, the mass fraction for obtaining chitosan solution is 1.5- 5%;
S6. silk gum aqueous solution is mixed with chitosan solution by 10: 0.05-0.3 mass ratio, and is added 1,2,3,4- Silk gum and chitosan blending surface is made in butane tetracarboxylic acid, sodium lauryl sulfate, catalyst, phytosterol, oxidizing glucose aldehyde Sizing agent is stirred and is kept the temperature at 60-70 DEG C spare.
Further, the molecule interception of bag filter is 10000-36000D in the step S2.
Further, the molecular weight of chitosan is 9 × 10 in the step S54-5×105
Further, 1,2,3,4- butane tetracarboxylic acid in the step S6, sodium lauryl sulfate, phytosterol aoxidize Portugal The additional amount of grape alditol and catalyst is respectively 1.5-3%, 0.1-0.6%, 0.5-1%, 1-2% and the 0.5-1% of solution quality.
Further, the step S6 catalyst is the mixture of trisodium citrate and sodium tartrate, mass ratio 1:2.
1. further, acetic acid solution concentration is 0.2 mol/L in the step S5.
Beneficial effect:Sizing agent of the invention has the following advantages that:
The moderate silk gum mixing of the chitosan and molecular weight that the present invention selects molecular weight moderate, because of the higher chitosan stream of molecular weight Dynamic property is poor, and the lower chitosan molecule of molecular weight is penetrated into after being glued in the interfiber pore of paper, and interfiber pore is more, fine Dimension table face film forming is poor, and silk gum will appear the irregular situation of sizing in Process of Applying Glue, therefore cooperation is made with phytosterol Sizing uniformly, while using crosslinking agent that glue and paper are bonded, and obtains the good sizing agent of sizability.
Specific embodiment
Embodiment 1
A kind of preparation method of silk gum paper sizing agent, includes the following steps:
S1. reeling mill is discarded into degumming liquid filtering, solution is placed in 60 DEG C of water-baths, is concentrated in vacuo;
S2. concentrate is put into bag filter, and the molecule interception of bag filter is 10000D, and dialysis is removed to metal ion, obtained To silk gum aqueous solution, silk gum then is obtained by filtration in silk gum aqueous solution;
S3. the dehydrated alcohol of 3 times of parts by weight is added in the silk gum prepared by step S2, filters 12h at 4 DEG C, must crystallize, uses Ethyl alcohol is washed again to be filtered again twice, dry under the conditions of 60 DEG C, obtains silk gum crystallization;
S4. silk gum is slowly dissolve into water, configures silk gum aqueous solution, the mass fraction for obtaining silk gum aqueous solution is 4%;
It S5. is 5 × 10 by molecular weight5Chitosan stirring and dissolving obtains chitosan solution in 0.2 mol/L acetic acid solution Mass fraction is 1.5%;
S6. silk gum aqueous solution is mixed with chitosan solution by 10: 0.05 mass ratio, and 1,2,3,4- butane is added Tetrabasic carboxylic acid, sodium lauryl sulfate, catalyst, phytosterol, oxidizing glucose aldehyde, is made silk gum and chitosan blending surface is glued Agent is stirred and is kept the temperature at 60-70 DEG C spare, wherein 1,2,3,4- butane tetracarboxylic acid, sodium lauryl sulfate, phytosterol, oxygen The additional amount for changing grape alditol and catalyst is respectively the 1.5%, 0.1%, 1%, 1% and 1% of solution quality, and catalyst is citric acid The mixture of trisodium and sodium tartrate, mass ratio 1:2.
Embodiment 2
A kind of preparation method of silk gum paper sizing agent, includes the following steps:
S1. reeling mill is discarded into degumming liquid filtering, solution is placed in 70 DEG C of water-baths, is concentrated in vacuo;
S2. concentrate is put into bag filter, and the molecule interception of bag filter is 36000D, and dialysis is removed to metal ion, obtained To silk gum aqueous solution, silk gum then is obtained by filtration in silk gum aqueous solution;
S3. the dehydrated alcohol of 6 times of parts by weight is added in the silk gum prepared by step S2, filters 12h at 4 DEG C, must crystallize, uses Ethyl alcohol is washed again to be filtered again twice, dry under the conditions of 70 DEG C, obtains silk gum crystallization;
S4. silk gum is slowly dissolve into water, configures silk gum aqueous solution, the mass fraction for obtaining silk gum aqueous solution is 8%;
It S5. is 9 × 10 by molecular weight4Chitosan stirring and dissolving obtains chitosan solution in 0.2 mol/L acetic acid solution Mass fraction is 5%;
S6. silk gum aqueous solution and chitosan solution are pressed 10:0.3 mass ratio is mixed, and 1,2,3,4- butane are added Tetrabasic carboxylic acid, sodium lauryl sulfate, catalyst, phytosterol, oxidizing glucose aldehyde, is made silk gum and chitosan blending surface is glued Agent is stirred and is kept the temperature at 60-70 DEG C spare, wherein 1,2,3,4- butane tetracarboxylic acid, sodium lauryl sulfate, phytosterol, oxygen The additional amount for changing grape alditol and catalyst is respectively the 3%, 0.6%, 0.5%, 2% and 0.5% of solution quality, and catalyst is lemon The mixture of sour trisodium and sodium tartrate, mass ratio 1:2.
Embodiment 3
A kind of preparation method of silk gum paper sizing agent, includes the following steps:
S1. reeling mill is discarded into degumming liquid filtering, solution is placed in 60 DEG C of water-baths, is concentrated in vacuo;
S2. concentrate is put into bag filter, and the molecule interception of bag filter is 15000D, and dialysis is removed to metal ion, obtained To silk gum aqueous solution, silk gum then is obtained by filtration in silk gum aqueous solution;
S3. the dehydrated alcohol of 4 times of parts by weight is added in the silk gum prepared by step S2, filters 12h at 4 DEG C, must crystallize, uses Ethyl alcohol is washed again to be filtered again twice, dry under the conditions of 60 DEG C, obtains silk gum crystallization;
S4. silk gum is slowly dissolve into water, configures silk gum aqueous solution, the mass fraction for obtaining silk gum aqueous solution is 5%;
It S5. is 9 × 10 by molecular weight4Chitosan stirring and dissolving obtains chitosan solution in 0.2 mol/L acetic acid solution Mass fraction is 2.5%;
S6. silk gum aqueous solution is mixed with chitosan solution by 10: 0.1 mass ratio, and 1,2,3,4- butane four is added Carboxylic acid, sodium lauryl sulfate, catalyst, phytosterol, oxidizing glucose aldehyde, is made silk gum and chitosan blending surface is glued Agent is stirred and is kept the temperature at 70 DEG C spare, wherein 1,2,3,4- butane tetracarboxylic acid, sodium lauryl sulfate, phytosterol, oxidation The additional amount of grape alditol and catalyst is respectively the 1.8%, 0.5%, 0.7%, 1.8% and 0.6% of solution quality, and catalyst is lemon The mixture of lemon acid trisodium and sodium tartrate, mass ratio 1:2.
Embodiment 4
A kind of preparation method of silk gum paper sizing agent, includes the following steps:
S1. reeling mill is discarded into degumming liquid filtering, solution is placed in 70 DEG C of water-baths, is concentrated in vacuo;
S2. concentrate is put into bag filter, and the molecule interception of bag filter is 30000D, and dialysis is removed to metal ion, obtained To silk gum aqueous solution, silk gum then is obtained by filtration in silk gum aqueous solution;
S3. the dehydrated alcohol of 5 times of parts by weight is added in the silk gum prepared by step S2, filters 12h at 4 DEG C, must crystallize, uses Ethyl alcohol is washed again to be filtered again twice, dry under the conditions of 70 DEG C, obtains silk gum crystallization;
S4. silk gum is slowly dissolve into water, configures silk gum aqueous solution, the mass fraction for obtaining silk gum aqueous solution is 7%;
It S5. is 5 × 10 by molecular weight5Chitosan stirring and dissolving obtains chitosan solution in 0.2 mol/L acetic acid solution Mass fraction is 4%;
S6. silk gum aqueous solution is mixed with chitosan solution by 10: 0.2 mass ratio, and 1,2,3,4- butane is added Tetrabasic carboxylic acid, sodium lauryl sulfate, catalyst, phytosterol, oxidizing glucose aldehyde, is made silk gum and chitosan blending surface is glued Agent is stirred and is kept the temperature at 65 DEG C spare, wherein 1,2,3,4- butane tetracarboxylic acid, sodium lauryl sulfate, phytosterol, oxidation The additional amount of grape alditol and catalyst is respectively the 2.4%, 0.2%, 0.9%, 1.2% and 0.9% of solution quality, and catalyst is lemon The mixture of lemon acid trisodium and sodium tartrate, mass ratio 1:2.
Embodiment 5
A kind of preparation method of silk gum paper sizing agent, includes the following steps:
S1. reeling mill is discarded into degumming liquid filtering, solution is placed in 65 DEG C of water-baths, is concentrated in vacuo;
S2. concentrate is put into bag filter, and the molecule interception of bag filter is 22000D, and dialysis is removed to metal ion, obtained To silk gum aqueous solution, silk gum then is obtained by filtration in silk gum aqueous solution;
S3. the dehydrated alcohol of 3-6 times of parts by weight is added in the silk gum prepared by step S2, filters 12h at 4 DEG C, must crystallize, It is washed with ethyl alcohol and is filtered again twice again, it is dry under the conditions of 65 DEG C, obtain silk gum crystallization;
S4. silk gum is slowly dissolve into water, configures silk gum aqueous solution, the mass fraction for obtaining silk gum aqueous solution is 7%;
It S5. is 3 × 10 by molecular weight5Chitosan stirring and dissolving obtains chitosan solution in 0.2 mol/L acetic acid solution Mass fraction is 3.5%;
S6. silk gum aqueous solution is mixed with chitosan solution by 10: 0.2 mass ratio, and 1,2,3,4- butane is added Tetrabasic carboxylic acid, sodium lauryl sulfate, catalyst, phytosterol, oxidizing glucose aldehyde, is made silk gum and chitosan blending surface is glued Agent is stirred and is kept the temperature at 65 DEG C spare, wherein 1,2,3,4- butane tetracarboxylic acid, sodium lauryl sulfate, phytosterol, oxidation The additional amount of grape alditol and catalyst is respectively the 2%, 0.4%, 0.8%, 1.5% and 0.8% of solution quality, and catalyst is lemon The mixture of sour trisodium and sodium tartrate, mass ratio 1:2.
Compound sizing agent is uniformly applied to body paper surface using coating machine, the paper after sizing is put on glazing drying machine and does Dry 3min obtains the paper after top sizing.Paper samples are placed in constant temperature and humidity(23 DEG C, RH=50%)Under the conditions of equilibrium water Test performance after point 24 h.
Surface strength of paper is measured according to 2679. 15-1997 of GB/T using printing adaptability analyzer;Utilize interlayer knot Resultant force tester tests paper internal bond strength according to GB/T 26203-2010;Using tensile strength tester according to GB/T 453-1989 measures paper tensile strength;Paper printing ink absorbability is measured according to GB/T 456-1989;Utilize Bekk formula smoothness Instrument measures paper smoothness according to GB/T 456-1989.
Note:Resin added is 1.5 ± 0.2gm2, comparative example 1 is pure chitosan sizing agent.

Claims (6)

1. a kind of preparation method of silk gum paper sizing agent, which is characterized in that include the following steps:
S1. reeling mill is discarded into degumming liquid filtering, solution is placed in 60-70 DEG C of water-bath, is concentrated in vacuo;
S2. concentrate is put into bag filter, and dialysis is removed to metal ion, obtains silk gum aqueous solution, then that silk gum is water-soluble Silk gum is obtained by filtration in liquid;
S3. the dehydrated alcohol of 3-6 times of parts by weight is added in the silk gum prepared by step S2, filters 12h at 4 DEG C, must crystallize, It is washed with ethyl alcohol and is filtered again twice again, it is dry under the conditions of 60-70 DEG C, obtain silk gum crystallization;
S4. silk gum is slowly dissolve into water, configures silk gum aqueous solution, the mass fraction for obtaining silk gum aqueous solution is 4-8%;
S5. by chitosan stirring and dissolving in acetic acid solution, the mass fraction for obtaining chitosan solution is 1.5-5%;
S6. silk gum aqueous solution is mixed with chitosan solution by 10: 0.05-0.3 mass ratio, and is added 1,2,3,4- Silk gum and chitosan blending surface is made in butane tetracarboxylic acid, sodium lauryl sulfate, catalyst, phytosterol, oxidizing glucose aldehyde Sizing agent is stirred and is kept the temperature at 60-70 DEG C spare.
2. a kind of preparation method of silk gum paper sizing agent according to claim 1, it is characterised in that:In the step S2 The molecule interception of bag filter is 10000-36000D.
3. a kind of preparation method of silk gum paper sizing agent according to claim 1, it is characterised in that:In the step S5 The molecular weight of chitosan is 9 × 104-5×105
4. a kind of preparation method of silk gum paper sizing agent according to claim 1, it is characterised in that:In the step S6 The additional amount of 1,2,3,4- butane tetracarboxylic acid, sodium lauryl sulfate, phytosterol, oxidizing glucose aldehyde and catalyst is respectively molten 1.5-3%, 0.1-0.6%, 0.5-1%, 1-2% and the 0.5-1% of liquid quality.
5. a kind of preparation method of silk gum paper sizing agent according to claim 1, it is characterised in that:The step S6 is urged Agent is the mixture of trisodium citrate and sodium tartrate, mass ratio 1:2.
6. a kind of preparation method of silk gum paper sizing agent according to claim 1, it is characterised in that:In the step S5 Acetic acid solution concentration is 0.2 mol/L.
CN201810811276.6A 2018-07-23 2018-07-23 A kind of preparation method of silk gum paper sizing agent Pending CN108867165A (en)

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Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB479110A (en) * 1936-04-27 1938-01-27 Talalay Anselm An improved process for making waterproof materials from paper, pasteboard, fabric and the like
CN1091785A (en) * 1993-01-20 1994-09-07 卡斯卡来·塞塔—菲拉彻·塞瑞彻·瑞尼特公司 Recovery method of sericin dissolved in degumming solution, equipment and sericin obtained therefrom
JPH1150397A (en) * 1997-06-03 1999-02-23 Hakusan Sangyo Kk Skin contact paper and its production
JPH1181185A (en) * 1997-09-04 1999-03-26 Hakusan Sangyo Kk Production of glossy paper
JP2002080498A (en) * 2000-09-05 2002-03-19 Hiroshi Akai Method for separating sericin and fibroin from wild silkworm cocoon such as cricula trifenestrata or the like and method for using separated sericin
JP2006182992A (en) * 2004-12-28 2006-07-13 Usm Kenkyusho:Kk Silk fine particle solution, method for producing silk fine particle powder, and material containing silk fine particle
CN104761616A (en) * 2015-04-15 2015-07-08 海安县南莫制丝有限公司 Method for preparing soluble silk protein liquid employing waste silk
CN105017382A (en) * 2015-08-14 2015-11-04 海安县南莫制丝有限公司 Method for preparing soluble silk protein solution through waste silk
CN105178108A (en) * 2015-09-21 2015-12-23 滁州卷烟材料厂 Manufacturing technology of aluminized paper for cigarettes
CN105968999A (en) * 2016-03-01 2016-09-28 阜阳市金木工艺品有限公司 Woodenware emulsion coating and manufacturing method thereof

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB479110A (en) * 1936-04-27 1938-01-27 Talalay Anselm An improved process for making waterproof materials from paper, pasteboard, fabric and the like
CN1091785A (en) * 1993-01-20 1994-09-07 卡斯卡来·塞塔—菲拉彻·塞瑞彻·瑞尼特公司 Recovery method of sericin dissolved in degumming solution, equipment and sericin obtained therefrom
JPH1150397A (en) * 1997-06-03 1999-02-23 Hakusan Sangyo Kk Skin contact paper and its production
JPH1181185A (en) * 1997-09-04 1999-03-26 Hakusan Sangyo Kk Production of glossy paper
JP2002080498A (en) * 2000-09-05 2002-03-19 Hiroshi Akai Method for separating sericin and fibroin from wild silkworm cocoon such as cricula trifenestrata or the like and method for using separated sericin
JP2006182992A (en) * 2004-12-28 2006-07-13 Usm Kenkyusho:Kk Silk fine particle solution, method for producing silk fine particle powder, and material containing silk fine particle
CN104761616A (en) * 2015-04-15 2015-07-08 海安县南莫制丝有限公司 Method for preparing soluble silk protein liquid employing waste silk
CN105017382A (en) * 2015-08-14 2015-11-04 海安县南莫制丝有限公司 Method for preparing soluble silk protein solution through waste silk
CN105178108A (en) * 2015-09-21 2015-12-23 滁州卷烟材料厂 Manufacturing technology of aluminized paper for cigarettes
CN105968999A (en) * 2016-03-01 2016-09-28 阜阳市金木工艺品有限公司 Woodenware emulsion coating and manufacturing method thereof

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Application publication date: 20181123