CN101033581A - Fire retardant for fabric and synthesis method thereof - Google Patents
Fire retardant for fabric and synthesis method thereof Download PDFInfo
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- CN101033581A CN101033581A CN 200710038826 CN200710038826A CN101033581A CN 101033581 A CN101033581 A CN 101033581A CN 200710038826 CN200710038826 CN 200710038826 CN 200710038826 A CN200710038826 A CN 200710038826A CN 101033581 A CN101033581 A CN 101033581A
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Abstract
This invention discloses a combination method for a flammable inhibitor of fabrics characterizing that a halogenated saturated fatty alcohol, P2O5 and dien react in the substantial ratio of 2 : 1 : 2 to prepare a flammable inhibitor, which is a multi-amine salt low polymer of haloalkylphosphate and includes three inhibitor elements of phosphor, nitrogen and halogen at the same time, its solution is in light yellow or orange and transparent, terylene, cotton or vinylon are good at inhibiting after they are cleaned up by said flammable inhibitor.
Description
Technical field
The present invention relates to a kind of fire retardant that is used for textile finishing and synthetic, be specifically related to a kind of fire retardant that is used for textile finishings such as terylene, cotton or polyvinyl.
Background technology
Fire retardant is that a class can stop polymeric material to ignite or suppresses the additive of flame propagation.The existing fire retardant that is used for dacron mainly contains phosphorus system, halogen system, inorganic system and the mixed system of several series wherein.Wherein, representative product is the Antiblaze1 9 that U.S. Mobil chemical company succeeded in developing in 1971 in the phosphorus flame retardant, and it is the mixture of mono phosphoric acid ester cyclic ester and phosphoric acid bicyclic diester, phosphorus content 21%; The FRC-1 that domestic like product has Changzhou Chemical Engineering Inst. to succeed in developing, this based flame retardant does not have flame retardant effect to fabrics such as cotton or polyvinyls, and it is more serious to carry out fabric moisture regain after the flame-proof treatment phenomenon that is clamminess.Halogenated flame retardant mainly is brominated and chloride compound, and commonly used has: the hexabromo-Cyclododecane (HBCD) of Beijing chemical fibre Research Institute, brominated amount 〉=70%; The deca-BDE (FR-10) of Tianjin synthetic material Research Institute; The trichloroethyl phosphate (TCEP) of Dongdu insecticide factory exploitation; The P5501 dacron fire retardant of Shanghai inorganic chemical industry Research Institute is the mixed system of bromine, antimony, and this based flame retardant is generally water insoluble, is not easy to the padding finishing of fabric.The mineral-type fire retardant mainly is used as the synergist of halogenated flame retardant based on antimony trioxide.Mainly contain N-dihydroxymethyl phosphono acrylamide (NMDPPA and be used for FLAME RETARDANT FOR COTTON CLOTH, be Pyrovatex CP) and Tetrakis hydroxymethyl phosphonium chloride (THPC or THPS), wherein Pyrovatex CP is the exploitation of Ciba Co., Ltd, and domestic like product has the FRC-2 of Changzhou Chemical Engineering Inst.; THPC is by the inferior (Albright﹠amp of Britain's Albright-Weir; Wilson) company develops nineteen fifty-five, and domestic also have like product to go on the market, and this based flame retardant contains free formaldehyde, and the fabric feeling after the arrangement hardens.
Thereby, a kind of fire retardant of new function admirable is provided, carry out the problem that the flame-proof treatment meeting causes fabric property to descend at present to solve, be the emphasis of current research; Simultaneously, both be applicable to that terylene was fire-retardant, be applicable to the fire retardant that cotton or polyvinyl are fire-retardant again, good effect will have been arranged for applying of product if can provide a kind of.
Summary of the invention
The object of the invention provides a kind of fire retardant that can be applicable to textile finishings such as terylene, cotton or polyvinyl simultaneously, and should not influence the feel of fabric after using.
For achieving the above object, the technical solution used in the present invention is: a kind of synthetic method that is used for the fire retardant of fabric, stir down phosphorus pentoxide is dropped in the halo saturated fatty alcohol, be cooled with circulating water, fully stir, after in 2～3 hours, having thrown phosphorus pentoxide, be warming up to 60～70 ℃ again, insulation reaction is 2～3 hours under this temperature, add diethylenetriamines then, and constantly stir, 90～110 ℃ of reactions 2～3 hours, be cooled to room temperature, add water according to needed solid content, fully stir the back and filter, filtrate is fire retardant, wherein, the ratio of the amount of substance of raw material is: halo saturated fatty alcohol: phosphorus pentoxide: diethylenetriamines=2: 1: 2.
In the technique scheme, described halo saturated fatty alcohol is represented X-C by following general formula
nH
2nOH, in the formula, n≤8, X=Cl or Br.
Further technical scheme is that described halo saturated fatty alcohol is selected from ethylene chlorhydrin, chloromethane alcohol, 2-chloropropyl alcohol, 3-chloropropyl alcohol, 2-methaform, 3-methaform, 4-methaform, 8-chlorine octanol, ethylene bromohyrin, 2-bromopropyl alcohol, 3-bromopropyl alcohol, 2-bromobutanol, 3-bromobutanol, 4-bromobutanol or 8-bromine octanol.
Wherein, optimized technical scheme is that described halo saturated fatty alcohol is an ethylene chlorhydrin.
The fire retardant that the simultaneously claimed employing said method of the present invention obtains; And this fire retardant is to the application in the flame-proof treatment of terylene, cotton or polyvinyl fabric.
The concrete implementing process of technique scheme can be: the halo saturated fatty alcohol is added in the reactor after than weighing by required amount of substance, start agitator, at normal temperatures phosphorus pentoxide is put in the reactor, and ON cycle water cooling, after in 2～3 hours, having thrown phosphorus pentoxide, be warming up to 60～70 ℃ again, insulation reaction is 2～3 hours under this temperature, then by required amount of substance than in reactor, adding diethylenetriamines, and constantly stir, 90～110 ℃ of reactions 2～3 hours, be cooled to room temperature, add a certain amount of water according to needed solid content, fully stir after 0.5 hour and filter, filtrate is product.This product is faint yellow or orange-yellow transparent liquid, and pH value is 6～7.
Because the technique scheme utilization, the present invention compared with prior art has following advantage:
1. the fire retardant of the present invention's acquisition is a kind of polyamines salt oligomer of halogenated alkyl phosphate, contain phosphorus, nitrogen, three kinds of ignition-proof elements of certain halogen simultaneously, it is faint yellow or orange-yellow and transparent that its aqueous solution is, fabrics such as terylene, cotton or polyvinyl had the good flame effect, there is not drip phenomenon during calcination, press GB/T 17595-1998 standard testing, fire resistance can reach B
1Level.
2. the fire retardant of the present invention's acquisition is to the not influence of feel of fabric.
3. technology of the present invention is simple, and course of reaction is convenient to control, is fit to suitability for industrialized production.
The specific embodiment
Below in conjunction with embodiment the present invention is further described:
Embodiment 1, with raw material ethylene chlorhydrin, phosphorus pentoxide and diethylenetriamines by amount of substance than being that weighing in 2: 1: 2 is good, again ethylene chlorhydrin is joined in the reactor, start agitator, at normal temperatures phosphorus pentoxide is put in the reactor, and the ON cycle water cooling, in 2 hours, thrown phosphorus pentoxide after, be warming up to 60 ℃ again, insulation reaction is 3 hours under this temperature.In reactor, add load weighted diethylenetriamines then, be warming up to 110 ℃, stir reaction down 2 hours.Add a certain amount of water again, fully stir after 0.5 hour and filter, filtrate is product.This product is faint yellow transparent liquid, and testing its solid content is 58.0%, and pH value is 6.5.Get the aqueous solution that this fire retardant is made into three groups of 200g/L, utilize it to put dacron, COTTON FABRIC, polyvinyl fabric respectively in order, it is as shown in table 1 to test its fire resistance by GB/T5455-1997 eqv ISO6941:1992 (mensuration of textile combustion performance vertical direction sample propagation of flame performance) method:
Fire resistance after table 1 terylene/cotton/polyvinyl textile finishing
| Char length (cm) | After flame time (s) | Duration of fire resistance (s) | |
| Dacron COTTON FABRIC polyvinyl fabric | 11.2 13.8 12.5 | 0 1.2 0 | 0 0 0 |
Embodiment 2, with raw material 2-chloropropyl alcohol, phosphorus pentoxide and diethylenetriamines by amount of substance than being that weighing in 2: 1: 2 is good, again the 2-chloropropyl alcohol is joined in the reactor, start agitator, at normal temperatures phosphorus pentoxide is slowly put in the reactor, and the ON cycle water cooling, in 3 hours, thrown phosphorus pentoxide after, be warming up to 70 ℃ again, insulation reaction is 2 hours under this temperature.In reactor, add load weighted diethylenetriamines then, be warming up to 100 ℃, stir reaction down 2.5 hours.Add a certain amount of water, fully stir after 0.5 hour and filter, filtrate is product.This product is faint yellow transparent liquid, and testing its solid content is 54.0%, and pH value is 6.0.Get the aqueous solution that this fire retardant is made into three groups of 200g/L, utilize it to put dacron, COTTON FABRIC, polyvinyl fabric respectively in order, it is as shown in table 2 to test its fire resistance by GB/T5455-1997 eqv ISO6941:1992 (mensuration of textile combustion performance vertical direction sample propagation of flame performance) method:
Fire resistance after table 2 terylene/cotton/polyvinyl textile finishing
| Char length (cm) | After flame time (s) | Duration of fire resistance (s) | |
| Dacron COTTON FABRIC polyvinyl fabric | 11.5 14.2 12.7 | 0 1.3 0 | 0 0 0 |
Embodiment 3, with raw material 8-chlorine octanol, phosphorus pentoxide and diethylenetriamines by amount of substance than being that weighing in 2: 1: 2 is good, again 8-chlorine octanol is joined in the reactor, start agitator, at normal temperatures phosphorus pentoxide is slowly put in the reactor, and the ON cycle water cooling, in 2.5 hours, thrown phosphorus pentoxide after, be warming up to 65 ℃ again, insulation reaction is 2.5 hours under this temperature.In reactor, add load weighted diethylenetriamines then, be warming up to 90 ℃, stir reaction down 3 hours.Add a certain amount of water again, fully stir after 0.5 hour and filter, filtrate is product.This product is faint yellow transparent liquid, and testing its solid content is 56.0%, and pH value is 6.6.Get the aqueous solution that this fire retardant is made into three groups of 200g/L, utilize it to put dacron, COTTON FABRIC, polyvinyl fabric respectively in order, it is as shown in table 3 to test its fire resistance by GB/T5455-1997 eqv ISO6941:1992 (mensuration of textile combustion performance vertical direction sample propagation of flame performance) method:
Fire resistance after table 3 terylene/cotton/polyvinyl textile finishing
| Char length (cm) | After flame time (s) | Duration of fire resistance (s) | |
| Dacron COTTON FABRIC polyvinyl fabric | 11.8 14.7 13.6 | 0 1.9 0 | 0 0 0 |
Embodiment 4, with raw material ethylene bromohyrin, phosphorus pentoxide and diethylenetriamines by amount of substance than being that weighing in 2: 1: 2 is good, again ethylene bromohyrin is joined in the reactor, start agitator, at normal temperatures phosphorus pentoxide is slowly put in the reactor, and the ON cycle water cooling, in 3 hours, thrown phosphorus pentoxide after, be warming up to 60 ℃ again, insulation reaction is 3 hours under this temperature.In reactor, add load weighted diethylenetriamines then, be warming up to 110 ℃, stir reaction down 2 hours.Add a certain amount of water, fully stir after 0.5 hour and filter, filtrate is product.This product is orange-yellow transparent liquid, and testing its solid content is 56.5%, and pH value is 6.2.Get the aqueous solution that this fire retardant is made into three groups of 200g/L, utilize it to put dacron, COTTON FABRIC, polyvinyl fabric respectively in order, it is as shown in table 4 to test its fire resistance by GB/T5455-1997 eqv ISO6941:1992 (mensuration of textile combustion performance vertical direction sample propagation of flame performance) method:
Fire resistance after table 4 terylene/cotton/polyvinyl textile finishing
| Char length (cm) | After flame time (s) | Duration of fire resistance (s) | |
| Dacron COTTON FABRIC polyvinyl fabric | 11.0 13.3 12.2 | 0 0.9 0 | 0 0 0 |
Embodiment 5, with raw material 2-bromopropyl alcohol, phosphorus pentoxide and diethylenetriamines by amount of substance than being that weighing in 2: 1: 2 is good, again the 2-bromopropyl alcohol is joined in the reactor, start agitator, at normal temperatures phosphorus pentoxide is slowly put in the reactor, and the ON cycle water cooling, in 2.5 hours, thrown phosphorus pentoxide after, be warming up to 70 ℃ again, insulation reaction is 2 hours under this temperature.In reactor, add load weighted diethylenetriamines then, be warming up to 100 ℃, stir reaction down 2.5 hours.Add a certain amount of water, fully stir after 0.5 hour and filter, filtrate is product.This product is orange-yellow transparent liquid, and testing its solid content is 60.0%, and pH value is 6.4.Get the aqueous solution that this fire retardant is made into three groups of 200g/L, utilize it to put dacron, COTTON FABRIC, polyvinyl fabric respectively in order, it is as shown in table 5 to test its fire resistance by GB/T5455-1997 eqv ISO6941:1992 (mensuration of textile combustion performance vertical direction sample propagation of flame performance) method:
Fire resistance after table 5 terylene/cotton/polyvinyl textile finishing
| Char length (cm) | After flame time (s) | Duration of fire resistance (s) | |
| Dacron COTTON FABRIC polyvinyl fabric | 10.6 13.1 11.8 | 0 0.8 0 | 0 0 0 |
Embodiment 6, with raw material 8-bromine octanol, phosphorus pentoxide and diethylenetriamines by amount of substance than being that weighing in 2: 1: 2 is good, again 8-bromine octanol is joined in the reactor, start agitator, at normal temperatures phosphorus pentoxide is slowly put in the reactor, and the ON cycle water cooling, in 2 hours, thrown phosphorus pentoxide after, be warming up to 65 ℃ again, insulation reaction is 2.5 hours under this temperature.In reactor, add load weighted diethylenetriamines then, be warming up to 90 ℃, stir reaction down 3 hours.Add a certain amount of water, fully stir after 0.5 hour and filter, filtrate is product.This product is orange-yellow transparent liquid, and testing its solid content is 58.5%, and pH value is 6.7.Get the aqueous solution that this fire retardant is made into three groups of 200g/L, utilize it to put dacron, COTTON FABRIC, polyvinyl fabric respectively in order, it is as shown in table 6 to test its fire resistance by GB/T5455-1997 eqv ISO6941:1992 (mensuration of textile combustion performance vertical direction sample propagation of flame performance) method:
Fire resistance after table 6 terylene/cotton/polyvinyl textile finishing
| Char length (cm) | After flame time (s) | Duration of fire resistance (s) | |
| Dacron COTTON FABRIC polyvinyl fabric | 10.2 13.0 11.6 | 0 1.4 0 | 0 0 0 |
Claims (6)
1. synthetic method that is used for the fire retardant of fabric, it is characterized in that: stir down phosphorus pentoxide is dropped in the halo saturated fatty alcohol, be cooled with circulating water, fully stir, after in 2～3 hours, having thrown phosphorus pentoxide, be warming up to 60～70 ℃ again, insulation reaction is 2～3 hours under this temperature, adds diethylenetriamines then, and constantly stir, 90～110 ℃ of reactions 2～3 hours, be cooled to room temperature, add water according to needed solid content, fully stirring the back filters, filtrate is fire retardant, and wherein, the ratio of the amount of substance of raw material is: halo saturated fatty alcohol: phosphorus pentoxide: diethylenetriamines=2: 1: 2.
2. the synthetic method that is used for the fire retardant of fabric according to claim 1 is characterized in that: described halo saturated fatty alcohol is represented X-C by following general formula
nH
2nOH, in the formula, n≤8, X=Cl or Br.
3. the synthetic method that is used for the fire retardant of fabric according to claim 2 is characterized in that: described halo saturated fatty alcohol is selected from ethylene chlorhydrin, chloromethane alcohol, 2-chloropropyl alcohol, 3-chloropropyl alcohol, 2-methaform, 3-methaform, 4-methaform, 8-chlorine octanol, ethylene bromohyrin, 2-bromopropyl alcohol, 3-bromopropyl alcohol, 2-bromobutanol, 3-bromobutanol, 4-bromobutanol or 8-bromine octanol.
4. the synthetic method that is used for the fire retardant of fabric according to claim 3 is characterized in that: described halo saturated fatty alcohol is an ethylene chlorhydrin.
5. adopt the fire retardant of the method acquisition of claim 1.
6. the fire retardant of claim 5 is to the application in the flame-proof treatment of terylene, cotton or polyvinyl fabric.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2007100388267A CN100494555C (en) | 2007-03-30 | 2007-03-30 | Fire retardant for fabric and synthesis method thereof |
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|---|---|---|---|
| CNB2007100388267A CN100494555C (en) | 2007-03-30 | 2007-03-30 | Fire retardant for fabric and synthesis method thereof |
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| CN101033581A true CN101033581A (en) | 2007-09-12 |
| CN100494555C CN100494555C (en) | 2009-06-03 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102400396A (en) * | 2010-09-07 | 2012-04-04 | 上海雅运纺织助剂有限公司 | Environmentally friendly fabric fire retardant and its preparation method and use |
| CN103074763A (en) * | 2012-12-28 | 2013-05-01 | 苏州市华智顾纺织有限公司 | Production method for flame-retardant cotton fabric |
| CN103074759A (en) * | 2013-01-14 | 2013-05-01 | 青岛大学 | Preparation method of metal ion flame retardant modification cotton fabric |
| CN103361976A (en) * | 2013-07-05 | 2013-10-23 | 吴江龙纺纺织有限公司 | Preparation method of anti-flaming modal fabric |
| CN103395263A (en) * | 2013-08-14 | 2013-11-20 | 苏州鑫汉纺纺织有限公司 | Novel dustproof shell fabric |
| CN106884212A (en) * | 2017-02-26 | 2017-06-23 | 浙江峰赫纺织有限公司 | A kind of flame vinylon fiber and preparation method thereof |
| CN107881773A (en) * | 2017-12-05 | 2018-04-06 | 苏州兆海纺织科技有限公司 | A kind of arrangement application process of phosphor nitrogen combustion inhibitor on dacron |
| CN116289195A (en) * | 2023-01-16 | 2023-06-23 | 苏州大学 | Flame-retardant polyester fabric based on phosphorus/nitrogen/boron flame-retardant system and preparation method thereof |
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2007
- 2007-03-30 CN CNB2007100388267A patent/CN100494555C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102400396A (en) * | 2010-09-07 | 2012-04-04 | 上海雅运纺织助剂有限公司 | Environmentally friendly fabric fire retardant and its preparation method and use |
| CN102400396B (en) * | 2010-09-07 | 2013-05-08 | 上海雅运纺织助剂有限公司 | Environmentally friendly fabric fire retardant and its preparation method and use |
| CN103074763A (en) * | 2012-12-28 | 2013-05-01 | 苏州市华智顾纺织有限公司 | Production method for flame-retardant cotton fabric |
| CN103074759A (en) * | 2013-01-14 | 2013-05-01 | 青岛大学 | Preparation method of metal ion flame retardant modification cotton fabric |
| CN103361976A (en) * | 2013-07-05 | 2013-10-23 | 吴江龙纺纺织有限公司 | Preparation method of anti-flaming modal fabric |
| CN103395263A (en) * | 2013-08-14 | 2013-11-20 | 苏州鑫汉纺纺织有限公司 | Novel dustproof shell fabric |
| CN106884212A (en) * | 2017-02-26 | 2017-06-23 | 浙江峰赫纺织有限公司 | A kind of flame vinylon fiber and preparation method thereof |
| CN106884212B (en) * | 2017-02-26 | 2019-08-06 | 浙江峰赫纺织有限公司 | A kind of flame vinylon fiber and preparation method thereof |
| CN107881773A (en) * | 2017-12-05 | 2018-04-06 | 苏州兆海纺织科技有限公司 | A kind of arrangement application process of phosphor nitrogen combustion inhibitor on dacron |
| CN116289195A (en) * | 2023-01-16 | 2023-06-23 | 苏州大学 | Flame-retardant polyester fabric based on phosphorus/nitrogen/boron flame-retardant system and preparation method thereof |
| CN116289195B (en) * | 2023-01-16 | 2024-02-09 | 苏州大学 | Flame-retardant polyester fabric based on phosphorus/nitrogen/boron flame-retardant system and preparation method thereof |
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| CN100494555C (en) | 2009-06-03 |
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Assignee: Hangzhou Meigao Huayi Chemical Co., Ltd. Assignor: Soochow University Contract fulfillment period: 2009.6.23 to 2015.6.22 contract change Contract record no.: 2009320001056 Denomination of invention: Fire retardant for fabric and synthesis method thereof Granted publication date: 20090603 License type: Exclusive license Record date: 2009.7.7 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.6.23 TO 2015.6.22; CHANGE OF CONTRACT Name of requester: HANGZHOU MEIGAO HUAYI CHEMICAL INDUSTRY CO., LTD. Effective date: 20090707 |
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Address after: Suzhou City, Jiangsu province 215137 Xiangcheng District Ji Road No. 8 Patentee after: Soochow University Address before: 215123 Suzhou City, Suzhou Province Industrial Park, No. love road, No. 199 Patentee before: Soochow University |
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Granted publication date: 20090603 Termination date: 20140330 |