CN103726338A - Preparation method of non-yellowing fluffing agent - Google Patents
Preparation method of non-yellowing fluffing agent Download PDFInfo
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- CN103726338A CN103726338A CN201310726684.9A CN201310726684A CN103726338A CN 103726338 A CN103726338 A CN 103726338A CN 201310726684 A CN201310726684 A CN 201310726684A CN 103726338 A CN103726338 A CN 103726338A
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- kilograms
- polyether modified
- methyl
- xanthochromia
- silicone oil
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- 238000004383 yellowing Methods 0.000 title abstract 4
- 238000002360 preparation method Methods 0.000 title abstract 2
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 27
- 229920000570 polyether Polymers 0.000 claims abstract description 27
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000000839 emulsion Substances 0.000 claims abstract description 20
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229960000583 acetic acid Drugs 0.000 claims abstract description 6
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000003921 oil Substances 0.000 claims description 28
- -1 fatty acyl amide compound Chemical class 0.000 claims description 23
- 235000010855 food raising agent Nutrition 0.000 claims description 22
- 230000000903 blocking effect Effects 0.000 claims description 17
- 239000001301 oxygen Substances 0.000 claims description 16
- 229910052760 oxygen Inorganic materials 0.000 claims description 16
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 8
- 238000004945 emulsification Methods 0.000 claims description 7
- 239000004593 Epoxy Substances 0.000 claims description 6
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 6
- QVYARBLCAHCSFJ-UHFFFAOYSA-N butane-1,1-diamine Chemical compound CCCC(N)N QVYARBLCAHCSFJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 4
- 230000006837 decompression Effects 0.000 claims description 4
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 2
- 238000009941 weaving Methods 0.000 claims description 2
- 229920002545 silicone oil Polymers 0.000 abstract description 14
- 239000004744 fabric Substances 0.000 abstract description 13
- 239000000126 substance Substances 0.000 abstract description 6
- 230000007547 defect Effects 0.000 abstract description 2
- 230000001804 emulsifying effect Effects 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 3
- 238000013329 compounding Methods 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 abstract 1
- 235000014113 dietary fatty acids Nutrition 0.000 abstract 1
- 229930195729 fatty acid Natural products 0.000 abstract 1
- 239000000194 fatty acid Substances 0.000 abstract 1
- 150000004665 fatty acids Chemical class 0.000 abstract 1
- 229920000642 polymer Polymers 0.000 abstract 1
- 230000008092 positive effect Effects 0.000 abstract 1
- 125000002924 primary amino group Chemical class [H]N([H])* 0.000 abstract 1
- 150000003376 silicon Chemical class 0.000 description 16
- 239000003643 water by type Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 4
- OBFQBDOLCADBTP-UHFFFAOYSA-N aminosilicon Chemical compound [Si]N OBFQBDOLCADBTP-UHFFFAOYSA-N 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000001680 brushing effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229940008099 dimethicone Drugs 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- XQSFXFQDJCDXDT-UHFFFAOYSA-N hydroxysilicon Chemical compound [Si]O XQSFXFQDJCDXDT-UHFFFAOYSA-N 0.000 description 2
- 210000002189 macula lutea Anatomy 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 150000003141 primary amines Chemical group 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 239000004131 EU approved raising agent Substances 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 238000007151 ring opening polymerisation reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Landscapes
- Silicon Polymers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Polyethers (AREA)
Abstract
The invention relates to a preparation method of a non-yellowing fluffing agent, belonging to the organic synthesis and high-molecular polymerization reactions in the fields of chemical industry and high polymer chemistry. The method is characterized by comprising the following steps: preparing methyl-terminated polyether modified silicone oil for the non-yellowing fluffing agent, emulsifying to obtain a methyl-terminated polyether modified silicone oil emulsion, and compounding with fatty acid amide compounds, glacial acetic acid and deionized water to obtain the non-yellowing fluffing agent. By adopting the technical scheme, the method provided by the invention has the advantages and positive effects that in the prepared methyl-terminated polyether modified silicone oil with a novel structure, a hydrophilic polyether group is introduced to the chemical structure, thus the methyl-terminated polyether modified silicone oil has self-emulsifying property and is very convenient to emulsify; the prepared silicone oil emulsion has stable properties such as high-temperature resistance, acid-base resistance and no demulsification; meanwhile, by adopting methyl to terminate silicone oil, the existence of primary amine on the silicone oil chain is replaced, and the defects such as yellow spots of the silicone oil emulsion on the fabric are avoided.
Description
Technical field
The present invention relates to a kind of manufacture method of not xanthochromia raising agent, belong to organic synthesis and macromolecular polymerization reaction in chemical industry and chemical field.
Background technology
In textile printing and dyeing industry, especially, in terylene dyeing and printing process, filament is processed into after grey cloth, need to pass through brushing process, obtains the fine and closely woven fine hair of Len req.Brushing process be by fabric by a series of fuzzing rollers that are surrounded by card-clothing, by the needle point of metallic card clothing, provoked the fiber of fabric, the hook generation fine hair of having no progeny, needs to add a large amount of raising agents in this course, makes on fabric lint fluffy, is convenient to plucking and processes.If do not add raising agent, will inevitably cause disconnected hair, fabric matte to have the cloth cover flaw phenomenons such as pinprick.At present, on market, be mainly by emulsions such as dimethicone, hydroxy silicon oil, amido silicon oils and fatty acyl amide compound is composite makes, and dimethicone, hydroxy-silicone-oil emulsion are extremely unstable, easily breakdown of emulsion, is easy on fabric, leave the flaws such as silicon spot, and amino silicon oil emulsion, owing to having primary amine groups in its chemical constitution, easily oxidation forms chromophoric group, thereby along with white fabrics or light fabric are placed for a long time, occurs macula lutea phenomenon.
The patent of invention of authorizing, name is called a kind of production technology of raising agent, the patent No. is 200810062043.7, in his technical scheme, adopt the first ring-opening polymerization of octamethylcy-clotetrasiloxane, prepare hydroxy silicon oil, by after its emulsification, with amino silicon oil emulsion or composite with Tissuemat E emulsion, make a kind of raising agent again.Although this technique is simple and convenient, hydroxy-silicone-oil emulsion is extremely unstable, and easily breakdown of emulsion floating oil leaves the flaws such as silicon spot on cloth cover, and amino silicon oil emulsion very easily causes xanthochromia on white or light fabric.
Summary of the invention
Technical problem to be solved by this invention is: a kind of manufacture method of not xanthochromia raising agent is provided, can solves deficiency of the prior art.
The technical solution adopted for the present invention to solve the technical problems is: the manufacture method that a kind of not xanthochromia raising agent is provided, it is characterized in that: first make not xanthochromia raising agent methyl blocking polyether modified silicon oil used, its emulsification is made to methyl blocking polyether modified silicon oil emulsion, then make a kind of not xanthochromia raising agent with fatty acyl amide compound, glacial acetic acid, deionized water are composite.
Described methyl blocking polyether modified silicon oil manufacturing technique, comprises the following steps:
(1). by 1,3-diglycidyl ether oxygen base propyl group-1,1,50～100 kilograms of 100～400 kilograms of 3,3-tetramethyl disiloxanes and butanediamine, in the solvent of 10～100 kilograms of isopropyl alcohols, at 20～100 ℃ of temperature, react 1～10 hour, obtain amino-terminated little molecule intermediate A;
(2). by 100～500 kilograms of 200～500 kilograms of above-mentioned intermediate A and end ring oxygen polyoxyethylene poly-oxygen propylene aethers, in isopropanol solvent, copolyreaction is 1～10 hour, obtains amino-terminated polyether modified silicon oil intermediate B; End ring oxygen polyoxyethylene poly-oxygen propylene aether molecular weight is that 200～1000, EO number is 0～20, and PO number is 0～20;
(3). by 50～500 kilograms of above-mentioned intermediate B and methyl polyoxyethylene epoxy radicals ether 30-200 kilogram, at 40～100 ℃ of temperature, react 3～10 hours, decompression distillation removes isopropanol solvent, obtains not xanthochromia raising agent methyl blocking polyether modified silicon oil; Methyl polyoxyethylene epoxy radicals ether molecular weight is that 100～1000, EO number is 0～20.
Get 100 kilograms of the above-mentioned methyl blocking polyether modified silicon oils making, add 6 kilograms, glacial acetic acid, 100～200 kilograms of deionized waters, by churned mechanically method emulsification, make the methyl blocking polyether modified silicon oil emulsion of desired content, add again 50～100 kilograms of fatty acyl amide compounds, 200～500 kilograms of deionized waters, make a kind of not xanthochromia raising agent.
Described fatty acyl amide compound is weaving film, and selected model is the commercially available fluffy film of RL-U2 or the instant type film of H-RT.
Owing to adopting technique scheme, advantage and good effect that the present invention has are: the methyl blocking polyether modified silicon oil of a kind of novel structure of preparing, in its chemical constitution, introduce hydrophilic polyether group, thereby there is automatic emulsifying performance, emulsification is very convenient, the silicone oil emulsion making, there is high temperature resistant, acid and alkali-resistance, breakdown of emulsion equistability energy not, adopt methyl by silicone oil end-blocking simultaneously, replace the existence of primary amine groups on silicone oil chain, avoided silicone oil emulsion on fabric, to leave the defects such as macula lutea.
The specific embodiment
Below in conjunction with embodiment, be described in further detail, but the present invention is not limited to following examples, without prejudice to spirit and scope of the invention in the situation that, those skilled in the art can make changes and improvements to the present invention, so that it is applicable to different service conditions.
Embodiment 1
(1). in the 1000L reactor of agitator, thermometer, vacuum recovered material is housed, add 1,3-diglycidyl ether oxygen base propyl group-1,300 kilograms of 1,3,3-tetramethyl disiloxanes, 60 kilograms of butanediamine, add 50 kilograms of isopropyl alcohols, at 82 ℃ of temperature, react 3 hours, obtain amino-terminated little molecule intermediate A.In the situation that stirring, adding molecular weight is 130 kilograms of 400 end ring oxygen polyoxyethylene poly-oxygen propylene aethers, continue reaction 7 hours, obtain amino-terminated polyether modified silicon oil intermediate B, be cooled to 60 ℃ below temperature, adding molecular weight is 60 kilograms, 200 methyl polyoxyethylene epoxy radicals ether, at 70 ℃ of temperature, reacts 5 hours, decompression removes isopropanol solvent, obtains methyl blocking polyether modified silicon oil.
(2). get 100 kilograms of the above-mentioned methyl blocking polyether modified silicon oils making, add 6 kilograms, glacial acetic acid, deionized water 120 kg, by churned mechanically method, emulsification makes the methyl blocking polyether modified silicon oil emulsion of desired content, then adds 50 kilograms of the fluffy films of RL-U2,260 kilograms of deionized waters, stir, make a kind of not xanthochromia raising agent.
Embodiment 2
(1). in the 1000L reactor of agitator, thermometer, vacuum recovered material is housed, add 1,3-diglycidyl ether oxygen base propyl group-1,400 kilograms of 1,3,3-tetramethyl disiloxanes, 80 kilograms of butanediamine, add 70 kilograms of isopropyl alcohols, at 75 ℃ of temperature, react 5 hours, obtain amino-terminated little molecule intermediate A.In the situation that stirring, adding molecular weight is 95 kilograms of 300 end ring oxygen polyoxyethylene poly-oxygen propylene aethers, continue reaction 6 hours, obtain amino-terminated polyether modified silicon oil intermediate B, be cooled to 60 ℃ below temperature, adding molecular weight is 80 kilograms, 300 methyl polyoxyethylene epoxy radicals ether, at 82 ℃ of temperature, reacts 4 hours, decompression removes isopropanol solvent, obtains methyl blocking polyether modified silicon oil.
(2). get 100 kilograms of the above-mentioned methyl blocking polyether modified silicon oils making, add 6 kilograms, glacial acetic acid, 160 kilograms of deionized waters, by churned mechanically method, emulsification makes the methyl blocking polyether modified silicon oil emulsion of desired content, then adds 70 kilograms of the instant type films of H-RT, 410 kilograms of deionized waters, stir, make a kind of not xanthochromia raising agent.
Claims (5)
1. the manufacture method of xanthochromia raising agent not, it is characterized in that: first make not xanthochromia raising agent methyl blocking polyether modified silicon oil used, its emulsification is made to methyl blocking polyether modified silicon oil emulsion, then make a kind of not xanthochromia raising agent with fatty acyl amide compound, glacial acetic acid, deionized water are composite.
2. the manufacture method of a kind of not xanthochromia raising agent according to claim 1, is characterized in that: described methyl blocking polyether modified silicon oil manufacturing technique, comprises the following steps:
(1). by 1,3-diglycidyl ether oxygen base propyl group-1,1,50～100 kilograms of 100～400 kilograms of 3,3-tetramethyl disiloxanes and butanediamine, in the solvent of 10～100 kilograms of isopropyl alcohols, at 20～100 ℃ of temperature, react 1～10 hour, obtain amino-terminated little molecule intermediate A;
(2). by 100～500 kilograms of 200～500 kilograms of above-mentioned intermediate A and end ring oxygen polyoxyethylene poly-oxygen propylene aethers, in isopropanol solvent, copolyreaction is 1～10 hour, obtains this B in the middle of amino-terminated polyether modified silicon oil;
(3). by 50～500 kilograms of above-mentioned intermediate B and methyl polyoxyethylene epoxy radicals ether 30-200 kilogram, at 40～100 ℃ of temperature, react 3～10 hours, decompression distillation removes isopropanol solvent, obtains not xanthochromia raising agent methyl blocking polyether modified silicon oil.
3. the manufacture method of a kind of not xanthochromia raising agent according to claim 1, is characterized in that: described fatty acyl amide compound is weaving film, and selected model is the commercially available fluffy film of RL-U2 or the instant type film of H-RT.
4. the manufacture method of a kind of not xanthochromia raising agent according to claim 2, is characterized in that: described end ring oxygen polyoxyethylene poly-oxygen propylene aether molecular weight is that 200～1000, EO number is 0～20, and PO number is 0～20.
5. the manufacture method of a kind of not xanthochromia raising agent according to claim 2, is characterized in that: described methyl polyoxyethylene epoxy radicals ether molecular weight is that 100～1000, EO number is 0～20.
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| CN201310726684.9A CN103726338B (en) | 2013-12-17 | 2013-12-17 | A kind of manufacture method of non yellowing raising agent |
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| CN201310726684.9A CN103726338B (en) | 2013-12-17 | 2013-12-17 | A kind of manufacture method of non yellowing raising agent |
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| CN103726338A true CN103726338A (en) | 2014-04-16 |
| CN103726338B CN103726338B (en) | 2015-11-25 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105111444A (en) * | 2015-08-25 | 2015-12-02 | 射阳天源化工有限公司 | Manufacturing method of brightening and smoothening agent |
| CN105401451A (en) * | 2015-12-24 | 2016-03-16 | 福建隆上超纤有限公司 | Production method of high-performance suede superfine fiber synthetic leather for clothing |
| CN111235893A (en) * | 2019-07-25 | 2020-06-05 | 浙江德彩新材料科技有限公司 | Organic silicon finishing agent and preparation method thereof |
| CN111235890A (en) * | 2019-07-25 | 2020-06-05 | 浙江德彩新材料科技有限公司 | Raising agent and preparation method thereof |
| CN111945433A (en) * | 2020-08-26 | 2020-11-17 | 广东宏昊化工有限公司 | Softener for after-finishing acrylic fiber-containing cloth and preparation method thereof |
| CN115652641A (en) * | 2022-10-13 | 2023-01-31 | 英德市东鸿化工科技有限公司 | Preparation method and application of raising agent |
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| CN101280520A (en) * | 2008-05-27 | 2008-10-08 | 建德市白沙化工有限公司 | Production process of raising agent |
| CN103073568A (en) * | 2012-07-10 | 2013-05-01 | 上海硅普化学品有限公司 | 1,3-diglycidoxypropyl-1,1,3,3-tetramethyldisiloxane preparation method |
| CN103351469A (en) * | 2013-05-31 | 2013-10-16 | 浙江安诺其助剂有限公司 | Preparation method of block silicone oil softener |
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2013
- 2013-12-17 CN CN201310726684.9A patent/CN103726338B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101280520A (en) * | 2008-05-27 | 2008-10-08 | 建德市白沙化工有限公司 | Production process of raising agent |
| CN103073568A (en) * | 2012-07-10 | 2013-05-01 | 上海硅普化学品有限公司 | 1,3-diglycidoxypropyl-1,1,3,3-tetramethyldisiloxane preparation method |
| CN103351469A (en) * | 2013-05-31 | 2013-10-16 | 浙江安诺其助剂有限公司 | Preparation method of block silicone oil softener |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105111444A (en) * | 2015-08-25 | 2015-12-02 | 射阳天源化工有限公司 | Manufacturing method of brightening and smoothening agent |
| CN105401451A (en) * | 2015-12-24 | 2016-03-16 | 福建隆上超纤有限公司 | Production method of high-performance suede superfine fiber synthetic leather for clothing |
| CN111235893A (en) * | 2019-07-25 | 2020-06-05 | 浙江德彩新材料科技有限公司 | Organic silicon finishing agent and preparation method thereof |
| CN111235890A (en) * | 2019-07-25 | 2020-06-05 | 浙江德彩新材料科技有限公司 | Raising agent and preparation method thereof |
| CN111945433A (en) * | 2020-08-26 | 2020-11-17 | 广东宏昊化工有限公司 | Softener for after-finishing acrylic fiber-containing cloth and preparation method thereof |
| CN115652641A (en) * | 2022-10-13 | 2023-01-31 | 英德市东鸿化工科技有限公司 | Preparation method and application of raising agent |
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| CN103726338B (en) | 2015-11-25 |
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Effective date of registration: 20180516 Address after: 224300 8 de FA Dong Road, Sheyang Economic Development Zone, Jiangsu Patentee after: SHEYANG TIANYUAN CHEMICAL INDUSTRY CO., LTD. Address before: 224300 de FA Dong Road, Sheyang County, Yancheng City, Jiangsu Province, No. 8 Patentee before: Xue Chengqiang |