CN106674356A - Preparation method of fire retardants containing fiber-based phosphatidic acid - Google Patents

Preparation method of fire retardants containing fiber-based phosphatidic acid Download PDF

Info

Publication number
CN106674356A
CN106674356A CN201611059290.2A CN201611059290A CN106674356A CN 106674356 A CN106674356 A CN 106674356A CN 201611059290 A CN201611059290 A CN 201611059290A CN 106674356 A CN106674356 A CN 106674356A
Authority
CN
China
Prior art keywords
phosphatidic acid
flame retardant
fibre
bearing base
cellulose ether
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201611059290.2A
Other languages
Chinese (zh)
Inventor
程聚光
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xuancheng City Trooyawn Refined Chemical Industry Co Ltd
Original Assignee
Xuancheng City Trooyawn Refined Chemical Industry Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xuancheng City Trooyawn Refined Chemical Industry Co Ltd filed Critical Xuancheng City Trooyawn Refined Chemical Industry Co Ltd
Priority to CN201611059290.2A priority Critical patent/CN106674356A/en
Publication of CN106674356A publication Critical patent/CN106674356A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B11/00Preparation of cellulose ethers
    • C08B11/20Post-etherification treatments of chemical or physical type, e.g. mixed etherification in two steps, including purification
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L25/00Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
    • C08L25/02Homopolymers or copolymers of hydrocarbons
    • C08L25/04Homopolymers or copolymers of styrene
    • C08L25/06Polystyrene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/04Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C08L27/06Homopolymers or copolymers of vinyl chloride
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18Fireproof paints including high temperature resistant paints
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03Polysaccharides or derivatives thereof
    • D06M15/05Cellulose or derivatives thereof
    • D06M15/09Cellulose ethers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30Flame or heat resistance, fire retardancy properties

Abstract

The invention belongs to the technical fields of phosphorus-based flame retardants and particularly relates to a preparation method of fire retardants containing fiber-based phosphatidic acid. The preparation method comprises the following steps: reacting diethylaminoethyl cellulose ether with 2-hydroxy-6-methoxy-benzaldehyde in a solvent to obtain an intermediate; then reacting the intermediate with phosphorus oxychloride, and carrying out processing treatment to obtain a product. Compared with the prior art, the preparation method disclosed by the invention has the following advantages that the fire retardants containing the fiber-based phosphatidic acid, prepared by the method disclosed by the invention, is high in contents of nitrogen and phosphorus, higher in molecular weight, excellent in fire retardant property and environment-friendly, and can be used for fire retardance of polyvinyl chloride, polystyrene, textiles, coating and the like; the preparation method is simple and is suitable for industrial popularization and use.

Description

A kind of preparation method of fibre-bearing base phosphatidic acid based flame retardant
Technical field
The invention belongs to phosphorus flame retardant technical field, and in particular to a kind of preparation of fibre-bearing base phosphatidic acid based flame retardant Method.
Background technology
As the fields such as the development of social economy, electronic apparatus material, automobile, skyscraper, communications and transportation are due to fire prevention Security needs, the material for being used forces needs fire-retardant, to reduce generation and the protection people life property safety of fire, And TCEP, TCPP and TDCP are the most common are in fire retardant, its three kinds of fire retardants are additive flame retardant, easy to use, Low price, with the very big market competitiveness, and phosphorus flame retardant volatility is big, heat resistance is not enough, fire retardant phosphorus content with Flame retardant effect is substantially directly proportional, accordingly, it would be desirable to be directed to problem above research phosphorus flame retardant.
The content of the invention
The purpose of the present invention is for existing problem, there is provided a kind of preparation side of fibre-bearing base phosphatidic acid based flame retardant Method.
The present invention is achieved by the following technical solutions:A kind of preparation method of fibre-bearing base phosphatidic acid based flame retardant, Comprise the following steps:
(1)By DEAE-cellulose ether and 2- hydroxyl -6- Methoxy-benzaldehydes with mol ratio 1:1 mixing adds reaction In kettle, and the solvent equivalent to 10 times of its gross weight is added, be to react 8 hours under conditions of 65-70 DEG C in temperature, obtain centre Material;
(2)35 DEG C are maintained the temperature at, POCl3 is added dropwise in above-mentioned gained middle material, persistently stir 4-6 hours, mixed Material;
(3)Basicity will be obtained after above-mentioned compound alkali cleaning, washing is neutral solution, and the solution is Jing after dehydration, concentration, drying To fibre-bearing base phosphatidic acid based flame retardant.
Used as further improvement of these options, the solvent is:Acetonitrile, dichloromethane, tetrahydrofuran, ethyl acetate Or any one in chloroform.
As further improvement of these options, the step(2)The usage amount of middle POCl3 is lignocaine second The 40% of base cellulose ether weight.
As further improvement of these options, the step(2)Catalyst is added dropwise while middle dropwise addition POCl3.
Used as further improvement of these options, the catalyst is isopropyl titanate, and addition is lignocaine second The 3% of base cellulose ether weight.
As further improvement of these options, the step(3)Drying temperature be 65-85 DEG C.
The present invention has compared to existing technology advantages below:The fibre-bearing base phosphatide acids that in the present invention prepared by method is fire-retardant Agent nitrogen and phosphorus content is high, and molecular weight is larger, and excellent flame retardancy is environmentally friendly, can be used for polyvinyl chloride, polystyrene, weaving Product, coating etc. it is fire-retardant, preparation method is simple, and suitable industrialization promotion is used.
Specific embodiment
Embodiment 1
A kind of preparation method of fibre-bearing base phosphatidic acid based flame retardant, comprises the following steps:
(1)By DEAE-cellulose ether and 2- hydroxyl -6- Methoxy-benzaldehydes with mol ratio 1:1 mixing adds reaction In kettle, and the dichloromethane equivalent to 10 times of its gross weight is added, be to react 8 hours under conditions of 65-70 DEG C in temperature, obtained Middle material;
(2)35 DEG C are maintained the temperature at, POCl3 is added dropwise in above-mentioned gained middle material, persistently stir 4-6 hours, mixed Material;
(3)It is neutral solution that basicity will be obtained after above-mentioned compound alkali cleaning, washing, and solution Jing dehydrations, concentration are in temperature Fibre-bearing base phosphatidic acid based flame retardant is obtained after drying under the conditions of 65-85 DEG C.
Wherein, the step(2)The usage amount of middle POCl3 is the 40% of DEAE-cellulose ether weight.
Embodiment 2
A kind of preparation method of fibre-bearing base phosphatidic acid based flame retardant, its step(1)Middle solvent is ethyl acetate, in the step (2)Isopropyl titanate is added dropwise while middle dropwise addition POCl3, addition is the 3% of DEAE-cellulose ether weight;Remove Above content is outer in the same manner as in Example 1.
Flame retardant performance to preparing is detected, and arranges control group, and fire retardant is by three chlorine monoxids in control group With DEAE-cellulose ether with 1:3 mixed in molar ratio be raw material, make according to a conventional method, detect its performance obtain with Lower result:
Table 1
Project Embodiment 1 Embodiment 2 Control group
Phosphorus content(%) 15.6 16.2 8.4
Nitrogen content(%) 8.5 8.7 7.5
500 DEG C of carbon yields(%) 46.7 45.2 26.3
5% decomposition temperature(℃) 315 304 272
Fire retardant carbon phosphorus content is higher in the present invention, while carbon yield also has corresponding rising, the decomposition temperature of fire retardant 5% is corresponding Raise, but under identical condition, the addition of catalyst reduces the decomposition temperature of certain 5%.

Claims (6)

1. a kind of preparation method of fibre-bearing base phosphatidic acid based flame retardant, it is characterised in that comprise the following steps:
(1)By DEAE-cellulose ether and 2- hydroxyl -6- Methoxy-benzaldehydes with mol ratio 1:1 mixing adds reaction In kettle, and the solvent equivalent to 10 times of its gross weight is added, be to react 8 hours under conditions of 65-70 DEG C in temperature, obtain centre Material;
(2)35 DEG C are maintained the temperature at, POCl3 is added dropwise in above-mentioned gained middle material, persistently stir 4-6 hours, mixed Material;
(3)Basicity will be obtained after above-mentioned compound alkali cleaning, washing is neutral solution, and the solution is Jing after dehydration, concentration, drying To fibre-bearing base phosphatidic acid based flame retardant.
2. a kind of as claimed in claim 1 preparation method of fibre-bearing base phosphatidic acid based flame retardant, it is characterised in that the solvent For:Any one in acetonitrile, dichloromethane, tetrahydrofuran, ethyl acetate or chloroform.
3. a kind of as claimed in claim 1 preparation method of fibre-bearing base phosphatidic acid based flame retardant, it is characterised in that the step (2)The usage amount of middle POCl3 is the 40% of DEAE-cellulose ether weight.
4. a kind of as claimed in claim 1 preparation method of fibre-bearing base phosphatidic acid based flame retardant, it is characterised in that the step (2)Catalyst is added dropwise while middle dropwise addition POCl3.
5. a kind of as claimed in claim 4 preparation method of fibre-bearing base phosphatidic acid based flame retardant, it is characterised in that the catalysis Agent is isopropyl titanate, and addition is the 3% of DEAE-cellulose ether weight.
6. a kind of as claimed in claim 1 preparation method of fibre-bearing base phosphatidic acid based flame retardant, it is characterised in that the step (3)Drying temperature be 65-85 DEG C.
CN201611059290.2A 2016-11-28 2016-11-28 Preparation method of fire retardants containing fiber-based phosphatidic acid Pending CN106674356A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201611059290.2A CN106674356A (en) 2016-11-28 2016-11-28 Preparation method of fire retardants containing fiber-based phosphatidic acid

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201611059290.2A CN106674356A (en) 2016-11-28 2016-11-28 Preparation method of fire retardants containing fiber-based phosphatidic acid

Publications (1)

Publication Number Publication Date
CN106674356A true CN106674356A (en) 2017-05-17

Family

ID=58866851

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201611059290.2A Pending CN106674356A (en) 2016-11-28 2016-11-28 Preparation method of fire retardants containing fiber-based phosphatidic acid

Country Status (1)

Country Link
CN (1) CN106674356A (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104356242A (en) * 2014-10-17 2015-02-18 中国林业科学研究院林产化学工业研究所 Halogen-free cellulose based phosphorus flame retardant and preparation method thereof
CN104371031A (en) * 2014-10-17 2015-02-25 中国林业科学研究院林产化学工业研究所 Cellulose-based nitrogen-phosphorus flame retardant and preparation method thereof
CN105085568A (en) * 2015-08-21 2015-11-25 浙江万盛股份有限公司 Preparation method of tri(2-chloroisopropyl)phosphate (TCPP)

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104356242A (en) * 2014-10-17 2015-02-18 中国林业科学研究院林产化学工业研究所 Halogen-free cellulose based phosphorus flame retardant and preparation method thereof
CN104371031A (en) * 2014-10-17 2015-02-25 中国林业科学研究院林产化学工业研究所 Cellulose-based nitrogen-phosphorus flame retardant and preparation method thereof
CN105085568A (en) * 2015-08-21 2015-11-25 浙江万盛股份有限公司 Preparation method of tri(2-chloroisopropyl)phosphate (TCPP)

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
于伟东 等: "《纺织物理第二版》", 30 September 2009, 东华大学出版社 *
朱锡锋: "《生物质热解原理与技术》", 30 September 2006, 中国科学技术大学出版社 *

Similar Documents

Publication Publication Date Title
CN101921407B (en) Bromine-containing pentaerythritol phosphoester retardant and preparation method thereof
CN101857805B (en) P-N type flame retardant and synthesis method thereof
CN104371031B (en) Cellulose-based nitrogen-phosphorus flame retardant and preparation method thereof
CN103214691B (en) Phosphorus-nitrogen expanding type flame retardant and preparation method thereof
CN103992293A (en) Preparation method for halogen-free flame retardant and flame retardant polyolefin composition thereof
CN102659959A (en) Preparation method of three-in-one intumescent fire retardant
CN102731548B (en) Triazine chloro-trissilicate compound and preparation method thereof
CN103373717B (en) A kind of preparation method of the low-polymerization-dammonium ammonium polyphosphate aqueous solution
CN102344510B (en) Preparation method of three-source-in-one expansion type fire retardant
CN101570518B (en) Preparation method for expansion type melamine hypophosphite fire retardant
CN102675372A (en) Ethylenediamine bicyclo-tetra methylenemelamine phosphonate compound and preparation method thereof
CN104610571A (en) Cardanol-based phosphatefire-retardant plasticizer and preparation method thereof
CN104356242B (en) Halogen-free cellulose based phosphorus flame retardant and preparation method thereof
CN106674356A (en) Preparation method of fire retardants containing fiber-based phosphatidic acid
CN101638421B (en) Preparation method of o-diaminobenzene phosphorylchloride condensed pentaerythritol ester
CN102604157B (en) Flame retardant and preparation method thereof
CN1807552A (en) Novel phosphor nitrogen composite combustion inhibitor
CN102964630A (en) Preparation method of fire retardant containing phosphorus
CN107286370A (en) A kind of nitrogen phosphorus flame retardant and preparation method thereof
CN106008397A (en) Preparation method of pyrophosphate piperazine
CN102977043A (en) Fire retardation agent melamine polyphosphate preparation method
CN107955845B (en) Preparation method of special formaldehyde-free intumescent flame retardant for leather
CN108276439B (en) Brominated phosphate flame retardant and preparation method thereof
CN105837631B (en) A kind of preparation method of phosphorous modified epoxy plasticizer and obtained plasticizer
CN106699804A (en) Production method of flame retardant for polyurethane foaming plastic

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20170517

RJ01 Rejection of invention patent application after publication