KR20020059315A - A manufacturing process of an incombustible composition - Google Patents
A manufacturing process of an incombustible composition Download PDFInfo
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- KR20020059315A KR20020059315A KR1020020034444A KR20020034444A KR20020059315A KR 20020059315 A KR20020059315 A KR 20020059315A KR 1020020034444 A KR1020020034444 A KR 1020020034444A KR 20020034444 A KR20020034444 A KR 20020034444A KR 20020059315 A KR20020059315 A KR 20020059315A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2201/00—Cellulose-based fibres, e.g. vegetable fibres
- D10B2201/01—Natural vegetable fibres
- D10B2201/02—Cotton
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
- D10B2331/04—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET]
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/04—Heat-responsive characteristics
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Abstract
본 발명은 합성섬유(특히 폴리에스텔 섬유)와 폴리에스텔 섬유 및 천연섬유(특히 면섬유 또는 섬유소 섬유)와의 혼방직물, 편직물, 이들의 부직포 등의 섬유 구조물의 난연 가공에 적합한 난연성 조성물의 제조방법에 관한 것이다.The present invention relates to a method for producing a flame retardant composition suitable for flame retardant processing of fiber structures such as blended fabrics, knitted fabrics, and nonwoven fabrics of synthetic fibers (particularly polyester fibers) and polyester fibers and natural fibers (particularly cotton fibers or fibrous fibers). will be.
본 발명에 따르면, 디시안디아미드와 물과 인산 반응에서 구아닐유리아인산염의 생성반응과, 디시안디아미드와 제1인산암모늄과 제2인산암모늄 반응에서 구아니딘인산염을 생성하는 1차 축합 반응과, 상기의 1차 축합 반응에서 미반응물의 잔존물을 암모니아수로써 중화시키고 구아니딘인산염을 생성하는 2차 중화 반응과, 상기 1차 축합 반응과 2차 중화 반응에서 생성된 구아니딘인산염을 수용해도를 증가시키기 위하여 포르마린을 부가 반응시켜서 메치롤구아니딘인산염을 완결시키는 3차 부가 반응으로 구성된 난연성 조성물의 제조방법이 제공된다.According to the present invention, the reaction of the production of guanyl urinate in the reaction of dicyandiamide with water and the first condensation reaction to produce guanidine phosphate in the reaction of dicyandiamide with ammonium monophosphate and diammonium phosphate; In order to increase the water solubility of the unreacted residues in the first condensation reaction of the reaction with ammonia water to produce guanidine phosphate, and to increase the water solubility of the guanidine phosphate produced in the first and second neutralization reactions. Provided is a method for preparing a flame retardant composition consisting of a tertiary addition reaction in which addition reaction is completed to complete metholguanidine phosphate.
Description
본 발명은 합성섬유(특히 폴리에스텔 섬유)와 폴리에스텔 섬유 및 천연섬유(특히 면섬유 또는 섬유소 섬유)와의 혼방직물, 편직물, 이들의 부직포 등의 섬유 구조물의 난연 가공에 적합한 난연성 조성물의 제조방법에 관한 것이다.The present invention relates to a method for producing a flame retardant composition suitable for flame retardant processing of fiber structures such as blended fabrics, knitted fabrics, and nonwoven fabrics of synthetic fibers (particularly polyester fibers) and polyester fibers and natural fibers (particularly cotton fibers or fibrous fibers). will be.
섬유의 난연 처리에는 여러가지 방법들이 있다. 종래의 섬유 구조물들의 난연가공에 사용되는 약제는 주로 인계, 질소계, 할로겐계 원자들을 함유하는 화합물로서, 요소-인산 또는 이들의 나트륨염, 암모늄염, 요소 또는 아민염, 브롬의 염, 유기염, 무기염, 금속산화물 또는 금속수산화물 그리고 유기계염화화합물계 등이 사용되고, 상기 약제들을 단독 처리 또는 조합처리하는 방법에 따라서 여러가지의 난연가공 섬유 구조물들이 개발되고 있다.There are various methods for flame retardant treatment of fibers. Agents used in flame retardant processing of conventional fiber structures are mainly compounds containing phosphorus, nitrogen, and halogen atoms, urea-phosphate or its sodium salt, ammonium salt, urea or amine salt, bromine salt, organic salt, Inorganic salts, metal oxides or metal hydroxides and organic chloride compounds and the like are used, and various flame retardant fiber structures have been developed according to a method of treating or combining the drugs alone.
그러나, 종래의 방법으로는 난연성을 만족시켜 준다고 하여도, 섬유 구조물 표면상부로 난연 약제가 돌출되거나 섬유직물 표면상의 백화현상을 일으켜서 섬유제품의 고유물성이나 섬유제품의 품질이 하락되는 문제점이 있고, 섬유 구조물의착색, 강도저하, 불쾌한 냄새의 발생, 촉감이 하락하는 결점이 있어서 우수한 섬유 구조물의 난연가공 약제로써 적합하지 못한 문제점이 있다.However, even if the conventional method satisfies the flame retardancy, there is a problem that the flame retardant drug protrudes on the surface of the fiber structure or whitening on the surface of the textile fabric, thereby deteriorating the intrinsic properties of the textile product and the quality of the textile product. There is a drawback that the coloring of the fiber structure, the decrease in strength, the generation of an unpleasant smell, the touch is deteriorated, there is a problem that is not suitable as a flame retardant agent of excellent fiber structure.
본 발명의 목적은 상기와 같은 종래의 문제점을 감안하여, 가격이 저렴하고 사용시 편리한 수용해성의 난연제와, 난연제 조성물의 농도가 고농도로써 사용시에 소량 사용하여 섬유 구조물의 고유 물성을 저해시키지 않는 난연제와, 섬유 구조물의 가공 제품에 2차적인 물리화학적 변화 현상인 백화 현상, 변색, 악취발생, 촉감변화, 강도저하 등이 없는 난연제 및 저장 안정성이 반영구적인 수용성 난연제를 조성할 수 있는 난연성 조성물의 제조 방법을 제공함에 있다.The object of the present invention is to provide a water-soluble flame retardant that is inexpensive and convenient for use in view of the above-described conventional problems, and a flame retardant that does not inhibit the inherent physical properties of the fiber structure by using a small amount of the flame retardant composition at a high concentration when used. Method for producing a flame retardant composition capable of forming a flame retardant without the secondary physicochemical change phenomena such as whitening, discoloration, odor generation, tactile change, decrease in strength and semi-permanent water-soluble flame retardant to the processed product of the fiber structure In providing.
이하 본 발명의 구성 및 작용을 상세히 설명하면 다음과 같다.Hereinafter, the configuration and operation of the present invention in detail.
본 발명은 디시안디아미드와 물과 인산 반응에서 구아닐유리아인산염의 생성반응과, 디시안디아미드와 제1인산암모늄과 제2인산암모늄 반응에서 구아니딘인산염을 생성하는 1차 축합 반응과, 상기의 1차 축합 반응에서 미반응물의 잔존물을 암모니아수로써 중화시키고 구아니딘인산염을 생성하는 2차 중화 반응과, 상기 1차 축합 반응과 2차 중화 반응에서 생성된 구아니딘인산염을 수용해도를 증가시키기 위하여 포르마린을 부가 반응시켜서 메치롤구아니딘인산염을 완결시키는 3차 부가 반응으로 구성된다.The present invention provides a reaction for the production of guanyluria phosphate in phosphate reaction with dicyandiamide and water, a first condensation reaction for producing guanidine phosphate in dicyandiamide, ammonium monophosphate and diammonium phosphate reaction, and 1 Secondary neutralization reaction to neutralize the unreacted residues with ammonia water in the first condensation reaction to form guanidine phosphate, and addition reaction of formarin to increase the water solubility of the guanidine phosphate produced in the first and second neutralization reactions. It consists of a tertiary addition reaction which completes metholguanidine phosphate.
상기 각 과정인 1차 축합 반응식은The first condensation reaction formula of each process is
H2NC(NH)NHㆍCN＋H2O＋H3PO4→H2NC(NH)NHCONHㆍH3PO4와,H 2 NC (NH) NH, CN + H 2 O + H 3 PO 4 → H 2 NC (NH) NHCONHH 3 PO 4 ,
H2NC(NH)NHㆍCN＋NH4ㆍHPO4＋(NH4)2HPO4→NH2C(NH)NH2ㆍH3PO4이고,H 2 NC (NH) NH, CN + NH 4 ㆍ HPO 4 + (NH 4 ) 2 HPO 4 → NH 2 C (NH) NH 2 ㆍ H 3 PO 4 ,
2차 중화 반응식은The second neutralization reaction
H2NC(NH)NHCONH2＋NH4OH＋H3PO4＋3H2O →(NH2C(NH)NH2)2＋H3PO4＋2NH3＋CO2이며,H 2 NC (NH) NHCONH 2 + NH 4 OH + H 3 PO 4 + 3H 2 O → (NH 2 C (NH) NH 2 ) 2 + H 3 PO 4 + 2NH 3 + CO 2 ,
3차 부가 반응식은The third addition scheme is
NH2ㆍC(NH)NH2ㆍH3PO4＋HCHO →HOH2CHNC(NH)NH2ㆍH3PO4이다.NH 2 · C (NH) NH 2 · H 3 PO 4 + HCHO → HOH 2 CHNC (NH) NH 2 · H 3 PO 4 .
상기와 같은 구성 및 반응식을 갖는 본 발명은 디시안디아미드, 인산과 제1인산암모늄, 제2인산암모늄, 물 등을 고온에서 반응시켜서 인산-구아니딘 축합물을 합성시킨 후 미반응의 산성의 인산 축합물을 암모니아수 또는 구아니딘 카보네이트로 중화 또는 제산 반응 시킨 후, 포르마린 부가 반응을 진행하여 수용해성 난연제 조성물을 완성시키는 방법이다.The present invention having the structure and the reaction scheme as described above is reacted with dicyandiamide, phosphoric acid and the first ammonium phosphate, diammonium phosphate, water and the like at high temperature to synthesize a phosphate-guanidine condensate, and then unreacted acidic phosphoric acid condensation After neutralizing or deoxidizing water with ammonia water or guanidine carbonate, a formaline addition reaction is performed to complete the water-soluble flame retardant composition.
디시안디아미드와 인산, 디시안디아미드와 인산염, 인산-구아니딘 화합물 등이 난연성을 가진 조성물이라는 것은 공지의 사실이다. 그러나, 이들 화합물 등은 수용액으로 조제할 시에 수용액 중의 용해 농도가 낮고, 용액의 안정도가 하락하여 침전물이 생성되고 난연성이 하락하며 제품의 균일한 난연성 물성이 낮고 상품적 가치가 낮음이 분명한 사실이다. 또한 사용시에 불안정한 수용액으로 불편한 점들이 많다.It is well known that dicyandiamide and phosphoric acid, dicyandiamide and phosphate, phosphoric acid-guanidine compounds and the like are flame retardant compositions. However, when these compounds and the like are prepared in an aqueous solution, it is obvious that the dissolution concentration in the aqueous solution is low, the stability of the solution decreases, precipitates are formed, the flame retardancy is decreased, the uniform flame retardant properties of the product are low, and the commercial value is low. . In addition, there are many inconveniences due to unstable aqueous solution in use.
상기와 같은 종래의 문제점을 본 발명에 의해 디시안디아미드, 인산과 이들암모늄염, 물과 고온에서 축합물을 합성시키고, 암모니아수 또는 구아니딘 카보네이트로써 중화 또는 제산 반응시키며, 포르마린으로 부가 반응 시켜서 된 중축합화합물이 수용해성이 상승되고 안정한 난연성 조성물이 된다.The polycondensation compound obtained by synthesizing condensates at a high temperature with dicyandiamide, phosphoric acid and these ammonium salts, water and the above-mentioned problems according to the present invention, neutralizing or deacidifying with ammonia water or guanidine carbonate, and addition reaction with formarin This water solubility is raised and it becomes a stable flame retardant composition.
종래의 문제점을 해결하는 상기와 같은 본 발명의 구체적인 방법은 물을 14부에서 33부 범위로 첨가하고, 디시안디아미드 8부, 제1인산암모늄을 17부에서 10부, 제2인산암모늄을 17부에서 10부 범위로 첨가하며, 인산을 11부에서 13부로 투입하여 온도 95℃~98℃ 범위에서 약 1시간 동안 축합 반응시키거나, 물을 14부, 디시안디아미드 8부, 인산 32부를 투입하고 전기의 조건에서 축합 반응을 약 1시간 동안 행한 후 구아니딘 카보네이트 13부 또는 암모니아수 9부에서 32부 범위로 중화 또는 제산 반응 후 온도 70℃~75℃에서 포르마린 11부에서 14부 첨가 후 부가 반응을 약 45분간 진행완료시키는 방법이다.The specific method of the present invention as described above to solve the conventional problem is added water in the range of 14 parts to 33 parts, 8 parts of dicyandiamide, 17 to 10 parts of ammonium monophosphate, 17 ammonium diphosphate Part is added in the range of 10 parts, and phosphoric acid is added from 11 parts to 13 parts for condensation reaction for about 1 hour at a temperature of 95 ° C. to 98 ° C., or 14 parts of water, 8 parts of dicyandiamide, and 32 parts of phosphoric acid are added. After the condensation reaction was carried out for about 1 hour under the above conditions, neutralization or antacid reaction was carried out in the range of 13 parts of guanidine carbonate or 9 parts to 32 parts of ammonia water, followed by addition of 14 parts of formarin at 14 ° C. to 70 ° C. to 75 ° C., followed by addition reaction. The process is completed for about 45 minutes.
상기의 조건에서 물이 14부 이하로 투입할 시에는 디시안디아미드의 고온에서의 첨가산가수분해반응이 진행되지 않아서 구아닐유리아포스페이트 생성이 되지 않아 본 발명의 목적에 부합되지 않고, 물이 33부 이상 범위의 첨가시에도 수용액의 농도가 하락하여 가공 후의 난연성이 좋지않게 된다. 또한 암모니아수, 구아니딘 카보네이트 첨가 반응으로 중화하지 않고 포르마린 부가반응이 진행된 합성품은 저장 안정성이 하락하여 수용해성이 불량하게 된다.When water is added at 14 parts or less under the above conditions, the addition acid hydrolysis reaction at a high temperature of dicyandiamide does not proceed, so that no production of guanyl urea phosphate does not occur. The concentration of the aqueous solution decreases even at the addition of more than the negative range, resulting in poor flame retardancy after processing. In addition, a synthetic product in which the formarin addition reaction proceeds without being neutralized by the addition of ammonia water or guanidine carbonate is deteriorated in storage stability and thus poor in water solubility.
제1인산암모늄과 제2인산암모늄이 첨가되어 반응완료시에는 난연성이 상승되기 본 발명의 난연성 조성물의 제조방법에는 제1인산암모늄과 제2인산암모늄이 상기의 첨가량으로 행함이 바람직하다.When the first ammonium phosphate and the second ammonium phosphate are added to increase the flame retardancy upon completion of the reaction, it is preferable that the first ammonium phosphate and the second ammonium phosphate are performed in the above-mentioned amounts in the method for preparing the flame retardant composition of the present invention.
본 발명의 제조방법 중 제2차 포르마린 부가반응 시행시에 반응시간 45분간이 합당하다. 본 발명의 제조방법의 시료중의 시험시료를 반응시간 15분, 30분, 45분, 60분의 시험시료를 확인한 결과, 반응시간 15분은 조성물 중에 상온 침전물이 형성되었고, 반응시간 30분은 조성물을 상온 이하로 냉각되었을 때에 침전물이 확인되었으며, 반응시간 45분 진행한 시료는 상온에서 냉각시켜도 침전물이 발견되지 않았고, 60분 시료도 이와 똑같이 발견되지 않았다. 따라서, 본 발명의 제조방법 중 2차 부가반응은 약 45분간 진행함이 바람직하다.In the preparation method of the present invention, the reaction time of 45 minutes at the time of carrying out the second formalin addition reaction is reasonable. As a result of confirming the test samples in the reaction method of 15 minutes, 30 minutes, 45 minutes, and 60 minutes in the test sample of the preparation method of the present invention, the reaction time was 15 minutes, and a room temperature precipitate was formed in the composition. Precipitation was confirmed when the composition was cooled to room temperature or less, and the sample which proceeded for 45 minutes of reaction time was not found even when cooled at room temperature, and the sample for 60 minutes was not found the same. Therefore, it is preferable that the secondary addition reaction proceeds for about 45 minutes in the production method of the present invention.
그리고, 본 발명의 난연성 조성물의 제조방법은 초기의 축합반응을 온도 95℃~98℃에서 약 1시간 반응시킨 후 냉각하여, 암모니아수 또는 구아니딘 카보네이트로 중화하고, 온도 75℃에서 약 45분간 포르마린 부가반응시키는 반응공정이 바람직하다.In the method for preparing a flame retardant composition of the present invention, the initial condensation reaction is reacted for about 1 hour at a temperature of 95 ° C. to 98 ° C., followed by cooling, neutralizing with ammonia water or guanidine carbonate, and formaline addition reaction at a temperature of 75 ° C. for about 45 minutes. The reaction process to make it preferable.
이하에서는 실시예에 따라 난연성 조성물의 작용을 더욱 상세히 설명하고자 하고, 실시예에서 사용되는 부는 중량 퍼센트를 나타내는 것이다.Hereinafter, the operation of the flame retardant composition according to the embodiment will be described in more detail, and the part used in the example indicates a weight percentage.
첫번째 실시예는 환류냉각기, 교반기, 온도계가 부착된 4구 플라스크에 물 33부, 디시안디아미드 8부, 제1인산암모늄 10부, 제2인산암모늄 10부, 인산 13부를 넣고 교반하면서 온도 95~98℃로 상승시킨 후 유지하면서 약 1시간 동안 축합 반응시키고, 이후 냉각하여 구아니딘 카보네이트 13부로 중화시키며, 포르마린 13부를 투입하여 온도 75℃에서 부가반응을 약 45분간 시킨 후 냉각시켜, 난연성 조성물을 완성시킨다.In the first embodiment, a four-necked flask equipped with a reflux condenser, agitator, and thermometer was provided with 33 parts of water, 8 parts of dicyandiamide, 10 parts of ammonium diphosphate, 10 parts of ammonium diphosphate, and 13 parts of phosphoric acid, followed by stirring. Condensation reaction for about 1 hour while maintaining after raising to 98 ℃, and then cooled to neutralize with 13 parts of guanidine carbonate, 13 parts of formarin was added to the addition reaction at a temperature of 75 ℃ for about 45 minutes and then cooled to complete the flame-retardant composition Let's do it.
상기 첫번째 실시예에서 완성된 난연성 조성물은 농도가 50％이고, 청명한수용액상으로서 반영구적으로 물성변화없이 12개월간 상온에서 저장할 경우 안정한 특성을 가지고, 포리에스텔 기모지에 가공할 경우 난연성 조성물 수용액을 물에 20~25％로 희석한 용액에 원단을 함침하고 부착률 70％로 하여 온도 180℃에서 3분간 건조 경화처리한다. 상기의 과정을 거친 가공포는 45℃ 맥켈바나법의 연소 시험한 결과 난연성이 우수하고, 가공포를 내후성 촉진시험기에서 20일간 가습건조시행한 결과 일광 견뢰도가 우수하며, 백화 현상도 없고 촉감변화도 없는 결과를 얻을 수 있었다.The flame retardant composition completed in the first embodiment has a concentration of 50%, and is a clear aqueous solution, and has a stable characteristic when stored at room temperature for 12 months without changing the physical properties semi-permanently, when processed in polyester brushed paper, the aqueous solution of the flame retardant composition in water 20 The solution diluted to ˜25% is impregnated with the original fabric, and dried and cured at a temperature of 180 ° C. for 3 minutes at an adhesion rate of 70%. The processed cloth after the above process was excellent in flame retardancy as a result of the combustion test of the McKelvana method at 45 ° C., and the processed cloth was humidified and dried for 20 days in an accelerated weathering tester, which showed excellent daylight fastness, no whitening phenomenon, and no change in touch. No results were obtained.
두번째 실시예는 환류기 냉각기, 교반기, 온도계가 부착된 4구 플라스크에 물 28부, 디시안디아미드 8부, 제1인산암모늄 17부, 제2인산암모늄 17부, 인산 11부를 넣고 교반하면서 온도 상승하여 온도 98~95℃에서 약 1시간 축합반응을 시행하고 냉각하여 암모니아수 9부를 첨가 중화시킨 후 포르마린 10부를 첨가하고 온도 75℃에서 45분간 부가 반응시킨 후 냉각하여 난연성 조성물을 완성시킨다.In the second embodiment, a four-necked flask equipped with a reflux condenser, a stirrer, and a thermometer includes 28 parts of water, 8 parts of dicyandiamide, 17 parts of ammonium phosphate, 17 parts of diammonium phosphate, and 11 parts of phosphate, and the temperature is increased while stirring. After condensation reaction was performed at a temperature of 98-95 ° C. for about 1 hour, and cooled to neutralize addition of 9 parts of ammonia water, 10 parts of formalin was added and 45 minutes of addition reaction at temperature of 75 ° C. to complete the flame retardant composition.
상기 두번째 실시예에서 완성된 조성물은 전기와 같은 조건에서 가공포 시험을 한 결과 동일한 시험 결과를 얻었다.In the second embodiment, the completed composition was subjected to the work cloth test under the same conditions as described above to obtain the same test results.
세번째 실시예는 한류 냉각기, 교반기, 온도계가 부착된 4구 플라스크에 물 14부, 디시안디아미드 8부, 인산 32부를 넣고 가열하여 교반하면서 온도 95~98℃에서 축합반응을 약 1시간 동안 진행 한 후 다시 냉각하고 암모니아수 32부를 넣고 중화시킨 후 포르마린 14부를 투입하고 다시 가열하여 온도 75℃에서 45분간 부가반응시킨 후 냉각하여 난연성 조성물을 완성시킨다.In the third embodiment, 14 parts of water, 8 parts of dicyandiamide and 32 parts of phosphoric acid were added to a four-necked flask equipped with a current-cooler, a stirrer, and a thermometer, followed by heating and stirring. After cooling again, neutralized with 32 parts of ammonia water, 14 parts of formalin were added and heated again, followed by 45 minutes of additional reaction at a temperature of 75 ° C., followed by cooling to complete a flame retardant composition.
상기 세번째 실시예의 조성물을 첫번째 실시예와 같이 가공포 시험을 행한결과 동일한 시험 결과를 얻었다.The same test results were obtained when the composition of the third example was subjected to the work cloth test as in the first example.
이와같이 된 본 발명은 수용해성이 뛰어나 사용이 편리한 효과가 있고, 고농도로서 소량 사용이 가능하여 섬유 구조물의 고유 물성을 해치지 않는 효과가 있으며, 가공 제품에 2차적인 물리화학적 변화 현상이 없는 특징으로 백화 현상이나 변색이나 악취발생이나 촉감변화나 강도저하 등이 예방되는 효과가 있고, 저장 안정성이 반영구적인 효과가 있다.Thus, the present invention has excellent water solubility and is easy to use, and can be used in small amounts at high concentrations, thereby not damaging the inherent physical properties of the fiber structure, and having no secondary physical and chemical changes in processed products. It is effective in preventing phenomenon, discoloration, odor generation, change of touch and strength, and storage stability is semi-permanent.
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| KR101257289B1 (en) * | 2010-11-02 | 2013-04-23 | 한국화학연구원 | Flame resistant composition containing Phosphor-Nitrogen compound and thermoplastic resin composition containing the same |
| CN104389166A (en) * | 2014-10-23 | 2015-03-04 | 吉林化工学院 | Preparation method for water-soluble intumescent flame retardant for acrylic fabric |
| KR102250275B1 (en) * | 2020-02-10 | 2021-05-07 | 김동길 | flame-retardant nonwoven fabric and manufacturing method thereof |
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| JPS61238791A (en) * | 1985-04-15 | 1986-10-24 | Chisso Corp | Water-soluble flame retardant and production thereof |
| JPS6187656A (en) * | 1985-09-30 | 1986-05-06 | Mitsui Toatsu Chem Inc | Preparation of aqueous solution of addition product of guanidine phosphate and formaldehyde |
| JPH0272902A (en) * | 1988-09-08 | 1990-03-13 | Dainippon Ink & Chem Inc | Noncombustible ligneous material |
| JPH02270547A (en) * | 1989-04-12 | 1990-11-05 | Dainippon Ink & Chem Inc | Fire retardant ligneous material |
| US5009964A (en) * | 1989-07-11 | 1991-04-23 | Osmose Wood Preserving, Inc. | Composition and process for imparting fire retardant properties and improved thermal stability to cellulosic materials |
| JP3112314B2 (en) * | 1991-09-20 | 2000-11-27 | 株式会社アズ | Chemicals for flame retardant wood, flame retardant wood and method of processing flame retardant wood |
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| KR101257289B1 (en) * | 2010-11-02 | 2013-04-23 | 한국화학연구원 | Flame resistant composition containing Phosphor-Nitrogen compound and thermoplastic resin composition containing the same |
| CN104389166A (en) * | 2014-10-23 | 2015-03-04 | 吉林化工学院 | Preparation method for water-soluble intumescent flame retardant for acrylic fabric |
| KR102250275B1 (en) * | 2020-02-10 | 2021-05-07 | 김동길 | flame-retardant nonwoven fabric and manufacturing method thereof |
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