CN100340713C - Multifunction environment-protection type durable fabric flame-retardant agent and producing method therefor - Google Patents
Multifunction environment-protection type durable fabric flame-retardant agent and producing method therefor Download PDFInfo
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- CN100340713C CN100340713C CNB2006100385851A CN200610038585A CN100340713C CN 100340713 C CN100340713 C CN 100340713C CN B2006100385851 A CNB2006100385851 A CN B2006100385851A CN 200610038585 A CN200610038585 A CN 200610038585A CN 100340713 C CN100340713 C CN 100340713C
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- 239000004744 fabric Substances 0.000 title claims abstract description 15
- 239000012757 flame retardant agent Substances 0.000 title abstract 2
- 238000000034 method Methods 0.000 title description 3
- 239000003063 flame retardant Substances 0.000 claims abstract description 15
- 239000000376 reactant Substances 0.000 claims abstract description 15
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 claims abstract description 12
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims abstract description 10
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- VONWDASPFIQPDY-UHFFFAOYSA-N dimethyl methylphosphonate Chemical compound COP(C)(=O)OC VONWDASPFIQPDY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 5
- -1 dimethyl methyl phosphonates Chemical class 0.000 claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 239000011574 phosphorus Substances 0.000 claims description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 abstract 2
- 230000007547 defect Effects 0.000 abstract 1
- 239000011541 reaction mixture Substances 0.000 abstract 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical class O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 8
- MCONGYNHPPCHSD-UHFFFAOYSA-N 3-dimethoxyphosphoryl-n-(hydroxymethyl)propanamide Chemical compound COP(=O)(OC)CCC(=O)NCO MCONGYNHPPCHSD-UHFFFAOYSA-N 0.000 description 4
- 235000019256 formaldehyde Nutrition 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical class OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- AKXUUJCMWZFYMV-UHFFFAOYSA-M tetrakis(hydroxymethyl)phosphanium;chloride Chemical compound [Cl-].OC[P+](CO)(CO)CO AKXUUJCMWZFYMV-UHFFFAOYSA-M 0.000 description 2
- 229920000877 Melamine resin Polymers 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 206010003549 asthenia Diseases 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- BGYKJFCTOLGZEN-UHFFFAOYSA-N chloro(tetrahydroxy)-lambda5-phosphane Chemical compound OP(O)(O)(O)Cl BGYKJFCTOLGZEN-UHFFFAOYSA-N 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000007730 finishing process Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229940080818 propionamide Drugs 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 238000009988 textile finishing Methods 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Fireproofing Substances (AREA)
Abstract
The present invention discloses a multifunction environment-protection type durable fabric flame-retardant agent which is manufactured by using pentaerythritol, phosphorus pentoxide, dimethyl methyl phosphonate, triphenyl phosphite and stannous octoate as raw materials. A production method of the present invention comprises the steps that the dimethyl methyl phosphonate is added in a reaction vessel and is heated to 50 to 55 DEG; the phosphorus pentoxide is added and reactants are heated to 90 to 95 DEG, and the temperature is preserved for 2 to 4 hours; the reactants are cooled to 50 to 55 DEG and are added with the triphenyl phosphite, and the temperature is preserved for 1 to 2 hours, reaction mixtures are heated to 65 to 75 DEG and are added with the pentaerythritol, the reactants are added with the stannous octoate, the reaction temperature is kept at 75 to 85 DEG, the temperature is preserved for 2 to 5 hours, and a finished product can be obtained. The present invention has the advantages of good environmental protection performance flame retardant property and durability and overcomes the defects of the prior art.
Description
Technical field:
The present invention relates to a kind of fire retardant and production method.
Background technology:
Around the flame-retarded technology of natural fabric, having developed some is applicable to the fire retardant and the corresponding technology of textile finishing both at home and abroad.Is representative as the agent of COTTON FABRIC durable flame-proof with the Pyrovatex CP of the Ciba company of the THPC of Britain Allbright andWilson company, Switzerland.THPC is a tetrahydroxy phosphorus chloride, might produce bischlormethyl ether in building-up process, and carcinogenic danger is arranged, and contains free formaldehyde, now forbids.Pyrovatex CP belongs to the phosphate compounds of methylol acyl ammonia, a large amount of free formaldehydes are arranged, in order to make itself and fibre chemistry crosslinked to obtain washability, during arrangement, also to use many melamine methylols class (as the HMM) crosslinking agent that contains formaldehyde, make the free formaldehyde content on the fabric of arrangement back very high,, and have follow-up formaldehyde to discharge problem greater than 0.3%.Homemade fire retardant CFR2201, FRC22, TLO2512 etc. all belong to this type of.The main component of Pyrovatex CP fire retardant is N-methylol-3-dimethoxy phosphoryl propionamide, and it contains active group-N-CH
2OH can make fabric produce durable fire resistance with cellulose crosslinked or by means of crosslinking agent and cellulose crosslinked formation covalent bond more than 150 ℃.Pyrovatex CP based flame retardant is as the COTTON FABRIC antiflaming finishing agent, flame retardant effect and good endurance, and few to the strength loss of fabric, feel is good, but has limited its development because of containing a large amount of free formaldehydes.
Summary of the invention:
The object of the present invention is to provide a kind of good environmental protection, the multifunction environment-protection type durable fabric fire retardant and the production method of fire resistance and good endurance.
Technical solution of the present invention is:
A kind of multifunction environment-protection type durable fabric fire retardant, it is characterized in that: the raw material by following composition by weight is made:
65～75 parts of pentaerythrites
135～150 parts of phosphorus pentoxides
135～150 parts of dimethyl methyl phosphonates
10～15 parts of triphenyl phosphites
0.2～0.8 part of stannous octoate.
A kind of production method of multifunction environment-protection type durable fabric fire retardant, it is characterized in that: in reactor, add dimethyl methyl phosphonate 135～150 weight portions, be heated to 50～55 ℃, add phosphorus pentoxide 135～150 weight portions then, and reactant is heated to 90～95 ℃, be incubated 2～4 hours; Reactant is cooled to 50～55 ℃, adds triphenyl phosphite 10～15 weight portions again, be incubated 1～2 hour; Reactant mixture is heated to 65～75 ℃, adds 65～75 parts of pentaerythrites; In reactant, add stannous octoate 0.2～0.8 weight portion, keep 75～85 ℃ of reaction temperatures, be incubated 2～5 hours, get product.
Good environmental protection of the present invention, fire resistance and good endurance have overcome the defective of prior art.
The invention will be further described below in conjunction with embodiment.
The specific embodiment:
In the reactor that agitator, thermometer, dropping funel, condenser are housed, add dimethyl methyl phosphonate 135～150 weight portions (example 135,142,150 weight portions), be heated to 50～55 ℃ (50 ℃, 52 ℃, 55 ℃ of examples), add phosphorus pentoxide 135～150 weight portions (example 135,142,150 weight portions) then, and reactant is heated to 90～95 ℃ (90,92,95 ℃ of examples), be incubated 2～4 hours (example 2,3,4 hours); Reactant is cooled to 50～55 ℃ (50 ℃, 52 ℃, 55 ℃ of examples), adds triphenyl phosphite 10～15 weight portions (example 10,13,15 weight portions) again, be incubated 1～2 hour (example 1,1.5,2 hours); Reactant mixture is heated to 65～75 ℃ (65 ℃, 70 ℃, 75 ℃ of examples), adds 65～75 parts of pentaerythrites (example 65,70,75 weight portions); In reactant, add stannous octoate 0.2～0.8 weight portion (example 0.2,0.5,0.8 weight portion), keep 75～85 ℃ of reaction temperatures (75 ℃, 80 ℃, 85 ℃ of examples), be incubated 2～5 hours (example 2,3,4,5 hours), get product.
After measured, the hydroxyl value of product is 122mgKOH/g, phosphorus content 20.5%, active constituent content 81.2%.
To the finishing technique that uses this fire retardant be:
Flame-proof finishing process: fire retardant 430g/L, citric acid and maleic acid were with 1: 1 proportional arrangement 120g/L, and inferior sodium phosphate 35g/L bakes 180s, 175 ℃ of temperature; Technology: pad (two soak two rolls pick-up 75%), oven dry (110 ℃, 4min), bake, to soap, oven dry is washed 50 times.
To not as follows through cloth specimen of washing and the sample test result who washes after 50 times:
| After flame time/s | Time/s glows | Char length/cm | Oxygen index (OI) | |
| Not washing | 0 | 0 | 15 | 30 |
| 50 washings | 0 | 0 | 17.5 | 28 |
Claims (2)
1, a kind of multifunction environment-protection type durable fabric fire retardant, it is characterized in that: the raw material by following composition by weight is made:
65～75 parts of pentaerythrites
135～150 parts of phosphorus pentoxides
135～150 parts of dimethyl methyl phosphonates
10～15 parts of triphenyl phosphites
0.2～0.8 part of stannous octoate.
2, a kind of production method of multifunction environment-protection type durable fabric fire retardant, it is characterized in that: in reactor, add dimethyl methyl phosphonate 135～150 weight portions, be heated to 50～55 ℃, add phosphorus pentoxide 135～150 weight portions then, and reactant is heated to 90～95 ℃, be incubated 2～4 hours; Reactant is cooled to 50～55 ℃, adds triphenyl phosphite 10～15 weight portions again, be incubated 1～2 hour; Reactant mixture is heated to 65～75 ℃, adds 65～75 parts of pentaerythrites; In reactant, add stannous octoate 0.2～0.8 weight portion, keep 75～85 ℃ of reaction temperatures, be incubated 2～5 hours, get product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100385851A CN100340713C (en) | 2006-03-03 | 2006-03-03 | Multifunction environment-protection type durable fabric flame-retardant agent and producing method therefor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100385851A CN100340713C (en) | 2006-03-03 | 2006-03-03 | Multifunction environment-protection type durable fabric flame-retardant agent and producing method therefor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1814903A CN1814903A (en) | 2006-08-09 |
| CN100340713C true CN100340713C (en) | 2007-10-03 |
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ID=36907246
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100385851A Expired - Fee Related CN100340713C (en) | 2006-03-03 | 2006-03-03 | Multifunction environment-protection type durable fabric flame-retardant agent and producing method therefor |
Country Status (1)
| Country | Link |
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| CN (1) | CN100340713C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103146023A (en) * | 2013-02-06 | 2013-06-12 | 北京东方美龙化工科技有限公司 | Efficient flame retardant aliphatic oligomeric phosphate/phosphonate ester and preparation method thereof |
| CN112796105A (en) * | 2020-12-31 | 2021-05-14 | 砾维(新乡)纺织有限公司 | Production process of pure cotton CP flame-retardant fabric |
| CN113089330B (en) * | 2021-05-13 | 2022-10-25 | 苏州联胜化学有限公司 | Polyester durable flame retardant and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA985820A (en) * | 1970-09-02 | 1976-03-16 | Arthur Dock Fon Toy | N,n-dialkyl, o,o'-bis(dihalopropyl)phosphoramidate fire retardants for polymers |
| CN1732232A (en) * | 2002-12-27 | 2006-02-08 | 宝理塑料株式会社 | flame retardant resin composition |
-
2006
- 2006-03-03 CN CNB2006100385851A patent/CN100340713C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA985820A (en) * | 1970-09-02 | 1976-03-16 | Arthur Dock Fon Toy | N,n-dialkyl, o,o'-bis(dihalopropyl)phosphoramidate fire retardants for polymers |
| CN1732232A (en) * | 2002-12-27 | 2006-02-08 | 宝理塑料株式会社 | flame retardant resin composition |
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| Publication number | Publication date |
|---|---|
| CN1814903A (en) | 2006-08-09 |
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| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: JIANGSU GEMEIGAO TECHNOLOGY DEVELOPMENT CO., LTD. Free format text: FORMER NAME: NANTONG KEXING CHEMICAL CO., LTD. |
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| CP01 | Change in the name or title of a patent holder |
Address after: 226000, Zhenxing Road, Nantong economic and Technological Development Zone, Jiangsu 19, China Patentee after: Jiangsu Gemei High-Tech Development Co., Ltd. Address before: 226000, Zhenxing Road, Nantong economic and Technological Development Zone, Jiangsu 19, China Patentee before: Nantong Kexing Chemical Industry Co., Ltd. |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20071003 Termination date: 20210303 |