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CN106084150A - A kind of trimellitic anhydride class polycarboxylate water-reducer - Google Patents

A kind of trimellitic anhydride class polycarboxylate water-reducer Download PDF

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Publication number
CN106084150A
CN106084150A CN201610402253.0A CN201610402253A CN106084150A CN 106084150 A CN106084150 A CN 106084150A CN 201610402253 A CN201610402253 A CN 201610402253A CN 106084150 A CN106084150 A CN 106084150A
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China
Prior art keywords
parts
reducer
acid
trimellitic
liquid
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Pending
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CN201610402253.0A
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Chinese (zh)
Inventor
白健
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Liuzhou Qiangwei Forging Factory
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Liuzhou Qiangwei Forging Factory
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Priority to CN201610402253.0A priority Critical patent/CN106084150A/en
Publication of CN106084150A publication Critical patent/CN106084150A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/06Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
    • C08F283/065Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/24Macromolecular compounds
    • C04B24/26Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B24/2605Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/32Polymers modified by chemical after-treatment
    • C08G65/329Polymers modified by chemical after-treatment with organic compounds
    • C08G65/331Polymers modified by chemical after-treatment with organic compounds containing oxygen
    • C08G65/332Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof
    • C08G65/3324Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof cyclic
    • C08G65/3326Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof cyclic aromatic
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/30Water reducers, plasticisers, air-entrainers, flow improvers

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Polyethers (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The invention discloses a kind of trimellitic acid class polycarboxylate water-reducer, belong to chemical field.It is made up of following raw material: trimellitic anhydride 7.8 10.2 parts, methyl allyl polyoxyethylene ether 105 120 parts, 10.5 12 parts of acrylic acid, hydrogen peroxide (30%) 0.36 0.43 part, 0.15 0.18 parts of L ascorbic acid, pyridine 0.08 0.12 parts, thioglycolic acid 0.42 0.50 parts, chloroform 60 80 parts.The trimellitic acid class polycarboxylate water-reducer of the offer of the present invention, with low cost, synthetic operation is simple, generates without bad by-product, and product pendant reactive group is more, can be effectively improved water reducer serviceability.

Description

A kind of trimellitic anhydride class polycarboxylate water-reducer
Technical field
The present invention relates to chemical field, be specifically related to a kind of trimellitic acid class polycarboxylate water-reducer.
Background technology
Poly carboxylic acid series water reducer just can produce preferable diminishing and reinforced effects with it, coagulate concrete when volume is relatively low Knot time effects is less, slump-retaining the most relative with cement/admixture adaptability preferable, to concrete shrinkage shadow Ring less (referring to generally increase drying shrinkage not too much), become the naphthalene system that continues, melamine system, fatty family and sulfamate based water reducer it After water reducer of new generation.Poly carboxylic acid series water reducer molecular structure is comb shape, with more active group on its main chain, such as carboxylic Acid groups (COOH), sulfonic acid group (SO3H), oh group (OH), poly-ethane oxygen groups ((CH2CH2O)m—R) Deng.The effect of cement is had nothing in common with each other by each group, as carboxylic acid group has preferable dispersibility and retarding effect;Sulfonic dispersion Property is good;Hydroxyl not only has deferred action, moreover it is possible to play the effect being impregnated with moistening;Poly-ethane epoxide class group has holding flowing The effect of property.Molecular Design becomes the first-selected direction of many scholar's research polycarboxylate water-reducer performance characteristics.
Summary of the invention
For above-mentioned, it is an object of the invention to provide a kind of modified version water reducer based on polycarboxylate water-reducer.
The concrete technical scheme that the present invention takes is:
A kind of trimellitic acid class polycarboxylate water-reducer, is prepared from by following raw material: trimellitic anhydride 7.8-10.2 part, methyl allyl polyoxyethylene ether 105-120 part, acrylic acid 10.5-12 part, hydrogen peroxide (30%) 0.36- 0.43 part, L-AA 0.15-0.18 part, pyridine 0.08-0.12 part, thioglycolic acid 0.42-0.50 part, chloroform 60-80 part.
Present invention also offers the preparation method of a kind of trimellitic acid class polycarboxylate water-reducer, comprise the following steps:
(1) weigh poly glycol monomethyl ether and maleic anhydride, put in 150ml there-necked flask, put into chloroform conduct Solvent.Being heated to 60 DEG C and stir, reacting 4 hours, cooling obtains white solid after removing solvent, obtains modified polymeric monomer;
(2) preparation A liquid (a certain amount of acrylic acid and distilled water) and B liquid (a certain amount of thioglycolic acid, L-AA And distilled water) stand-by.Inserting thermometer on former there-necked flask, stirring to the polymeric monomer that heats up is completely dissolved, and instills hydrogen peroxide also Stir, be simultaneously added dropwise A liquid and B liquid with constant pressure funnel.It is incubated 1-2 hour after dropping.With 40% after cooling NaOH solution is neutralized to PH=6.0-7.0.
The trimellitic acid class polycarboxylate water-reducer that the present invention provides is the most with low cost, easy and simple to handle, without bad by-product Thing generates, and product pendant reactive group is more, can be effectively improved water reducer serviceability.
Detailed description of the invention
Below presently preferred embodiments of the present invention is described in detail so that advantages and features of the invention can be easier to by It will be appreciated by those skilled in the art that thus protection scope of the present invention is made apparent clear and definite defining.
Embodiment 1
A kind of trimellitic anhydride class polycarboxylate water-reducer, is prepared from by following raw material: trimellitic anhydride 7.8 parts, methyl allyl polyoxyethylene ether 105 parts, 10.5 parts of acrylic acid, hydrogen peroxide (30%) 0.36 part, L-AA 0.15 part, pyridine 0.08 part, thioglycolic acid 0.42 part, chloroform 60 parts.
Its concrete manufacturing process comprises the steps of
(1) weigh methyl allyl polyoxyethylene ether and trimellitic anhydride, put in 150ml there-necked flask, put into three Chloromethanes, as solvent, instills pyridine as catalyst.Being heated to 60 DEG C and stir, reacting 4 hours, cooling obtains after removing solvent White solid, obtains modified polymeric monomer;
(2) preparation A liquid (a certain amount of acrylic acid and distilled water) and B liquid (a certain amount of thioglycolic acid, L-AA And distilled water) stand-by.Inserting thermometer on former there-necked flask, stirring to the polymeric monomer that heats up is completely dissolved, and instills hydrogen peroxide also Stir, be simultaneously added dropwise A liquid and B liquid with constant pressure funnel.It is incubated 1-2 hour after dropping.With 40% after cooling NaOH solution is neutralized to PH=6.0-7.0.
Embodiment 2
A kind of trimellitic anhydride class polycarboxylate water-reducer, is prepared from by following raw material: trimellitic anhydride 9 Part, methyl allyl polyoxyethylene ether 112.5 parts, 11.25 parts of acrylic acid, hydrogen peroxide (30%) 0.395 part, L-AA 0.165 part, pyridine 0.10 part, thioglycolic acid 0.46 part, chloroform 70 parts.
Its concrete manufacturing process comprises the steps of
(1) weigh methyl allyl polyoxyethylene ether and trimellitic anhydride, put in 150ml there-necked flask, put into three Chloromethanes, as solvent, instills pyridine as catalyst.Being heated to 60 DEG C and stir, reacting 4 hours, cooling obtains after removing solvent White solid, obtains modified polymeric monomer;
(2) preparation A liquid (a certain amount of acrylic acid and distilled water) and B liquid (a certain amount of thioglycolic acid, L-AA And distilled water) stand-by.Inserting thermometer on former there-necked flask, stirring to the polymeric monomer that heats up is completely dissolved, and instills hydrogen peroxide also Stir, be simultaneously added dropwise A liquid and B liquid with constant pressure funnel.It is incubated 1-2 hour after dropping.With 40% after cooling NaOH solution is neutralized to PH=6.0-7.0.
Embodiment 3
A kind of trimellitic anhydride class polycarboxylate water-reducer, is prepared from by following raw material: trimellitic anhydride 10.2 parts, methyl allyl polyoxyethylene ether 120 parts, 12 parts of acrylic acid, hydrogen peroxide (30%) 0.43 part, L-AA 0.18 Part, pyridine 0.12 part, thioglycolic acid 0.50 part, chloroform 80 parts.
Its concrete manufacturing process comprises the steps of
(1) weigh methyl allyl polyoxyethylene ether and trimellitic anhydride, put in 150ml there-necked flask, put into three Chloromethanes, as solvent, instills pyridine as catalyst.Being heated to 60 DEG C and stir, reacting 4 hours, cooling obtains after removing solvent White solid, obtains modified polymeric monomer;
(2) preparation A liquid (a certain amount of acrylic acid and distilled water) and B liquid (a certain amount of thioglycolic acid, L-AA And distilled water) stand-by.Inserting thermometer on former there-necked flask, stirring to the polymeric monomer that heats up is completely dissolved, and instills hydrogen peroxide also Stir, be simultaneously added dropwise A liquid and B liquid with constant pressure funnel.It is incubated 1-2 hour after dropping.With 40% after cooling NaOH solution is neutralized to PH=6.0-7.0.

Claims (4)

1. a trimellitic acid class polycarboxylate water-reducer, it is characterised in that by weight, be made up of following raw material: benzene three partially Formic anhydride 7.8-10.2 part, methyl allyl polyoxyethylene ether 105-120 part, acrylic acid 10.5-12 part, hydrogen peroxide (30%) 0.36-0.43 part, L-AA 0.15-0.18 part, pyridine 0.08-0.12 part, thioglycolic acid 0.42-0.50 part, trichlorine Methane 60-80 part.
Trimellitic acid class polycarboxylate water-reducer the most according to claim 1, it is characterised in that by weight, by following Raw material forms: trimellitic anhydride 8.4-9.6 part, methyl allyl polyoxyethylene ether 110-115 part, acrylic acid 10.8-11.7 Part, hydrogen peroxide (30%) 0.38-0.41 part, L-AA 0.16-0.17 part, pyridine 0.09-0.11 part, thioglycolic acid 0.44-0.48 part, chloroform 65-75 part.
Trimellitic acid class polycarboxylate water-reducer the most according to claim 1, it is characterised in that by weight, by following Raw material forms: trimellitic anhydride 9 parts, methyl allyl polyoxyethylene ether 112.5 parts, 11.25 parts of acrylic acid, hydrogen peroxide (30%) 0.395 part, L-AA 0.165 part, pyridine 0.10 part, thioglycolic acid 0.46 part, chloroform 70 parts.
4. the preparation method of a trimellitic acid class polycarboxylate water-reducer, it is characterised in that comprise the following steps:
(1) weigh methyl allyl polyoxyethylene ether and trimellitic anhydride, put in 150ml there-necked flask, put into three chloromethanes Alkane, as solvent, instills pyridine as catalyst.Being heated to 60 DEG C and stir, reacting 4 hours, cooling obtains white after removing solvent Solid, obtains modified polymeric monomer;
(2) preparation A liquid (a certain amount of acrylic acid and distilled water) and B liquid (a certain amount of thioglycolic acid, L-AA and steaming Distilled water) stand-by.Inserting thermometer on former there-necked flask, stirring to the polymeric monomer that heats up is completely dissolved, and instills hydrogen peroxide and stirs Uniformly, it is simultaneously added dropwise A liquid and B liquid with constant pressure funnel.It is incubated 1-2 hour after dropping.Use 40%NaOH molten after cooling Liquid is neutralized to PH=6.0-7.0.
CN201610402253.0A 2016-06-08 2016-06-08 A kind of trimellitic anhydride class polycarboxylate water-reducer Pending CN106084150A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104140503A (en) * 2014-07-30 2014-11-12 江西格雷斯科技股份有限公司 Method for synthesizing high-water-reduction high-slump-retaining high-performance polycarboxylate water reducer at normal temperature
CN104926183A (en) * 2015-05-27 2015-09-23 中交四航工程研究院有限公司 High-adaptability and high-performance polycarboxylic water-reducing agent and preparation method for same
CN104961376A (en) * 2015-06-25 2015-10-07 贵州省瓮安新源新材料有限公司 Polycarboxylic acid high-performance water reducing agent and preparing method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104140503A (en) * 2014-07-30 2014-11-12 江西格雷斯科技股份有限公司 Method for synthesizing high-water-reduction high-slump-retaining high-performance polycarboxylate water reducer at normal temperature
CN104926183A (en) * 2015-05-27 2015-09-23 中交四航工程研究院有限公司 High-adaptability and high-performance polycarboxylic water-reducing agent and preparation method for same
CN104961376A (en) * 2015-06-25 2015-10-07 贵州省瓮安新源新材料有限公司 Polycarboxylic acid high-performance water reducing agent and preparing method thereof

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Application publication date: 20161109