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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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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| Application Number | Title | Priority Date | Filing Date |
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| 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 |
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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 |
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| CN1814903A (en) | 2006-08-09 |
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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 |