CN107325235A - One kind protects the sustained-release polycarboxylic water reducer normal temperature synthesis technique that collapses - Google Patents

One kind protects the sustained-release polycarboxylic water reducer normal temperature synthesis technique that collapses Download PDF

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Publication number
CN107325235A
CN107325235A CN201710575903.6A CN201710575903A CN107325235A CN 107325235 A CN107325235 A CN 107325235A CN 201710575903 A CN201710575903 A CN 201710575903A CN 107325235 A CN107325235 A CN 107325235A
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CN
China
Prior art keywords
parts
sustained
step
reaction vessel
hydrogen peroxide
Prior art date
Application number
CN201710575903.6A
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Chinese (zh)
Inventor
广禹华
广孝林
Original Assignee
贵州禹华建材科技有限公司
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Priority to CN201710575903.6A priority Critical patent/CN107325235A/en
Publication of CN107325235A publication Critical patent/CN107325235A/en

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Classifications

    • 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
    • C04B24/2688Copolymers containing at least three different monomers
    • C04B24/2694Copolymers containing at least three different monomers containing polyether side chains
    • 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
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/30Water reducers, plasticisers, air-entrainers, flow improvers
    • C04B2103/302Water reducers

Abstract

The sustained-release polycarboxylic water reducer normal temperature synthesis technique that collapses is protected the invention discloses one kind, is comprised the following steps:Step 1: adding bottom water, 10 35 DEG C of water temperature in reaction vessel;Methyl allyl polyoxyethylene ether is added into reaction vessel;Step 2: adding hydrogen peroxide in the reaction vessel of step one, crossing ammonium, and stir 35 minutes;Step 3: control reaction vessel interior temperature is between 10 35 DEG C, A gobs add 2.5 3.0 hours, and B gobs add 3.0 3.5 hours.It is proposed by the present invention it is a kind of protect the sustained-release polycarboxylic water reducer normal temperature synthesis technique that collapses, collapsed sustained-release polycarboxylic water reducer manufacturing process relative to tradition guarantor, preparation method is simple, easy to operate, road provided for a large amount of productions for protecting the sustained-release polycarboxylic water reducer that collapses.

Description

One kind protects the sustained-release polycarboxylic water reducer normal temperature synthesis technique that collapses

Technical field

Synthesized the present invention relates to technical field of chemical synthesis, more particularly to a kind of sustained-release polycarboxylic water reducer normal temperature that collapses of protecting Technique.

Background technology

Polycarboxylate water-reducer is a kind of high-performance water reducing agent, is a kind of cement dispersants during cement concrete is used.Extensively It is general to be applied to the engineerings such as highway, bridge, dam, tunnel, skyscraper.The product environmental protection, nonflammable, non-explosive, Ke Yian It is complete to use train and Automobile Transportation.

Traditional making protects when collapsing sustained-release polycarboxylic water reducer that technique is cumbersome, it is impossible to improves guarantor's sustained-release polycarboxylic that collapses and subtracts The yield of aqua, therefore, it is proposed that a kind of protect the sustained-release polycarboxylic water reducer normal temperature synthesis technique that collapses.

The content of the invention

The invention aims to solve shortcoming present in prior art, and the one kind proposed protects the poly- carboxylic of spacetabs type that collapses Sour water-reducer at normal temperature synthesis technique.

To achieve these goals, present invention employs following technical scheme:One kind protects the sustained-release polycarboxylic water reducer that collapses Normal temperature synthesis technique, comprises the following steps:

Step 1: adding bottom water, 10-35 DEG C of water temperature in reaction vessel;Methacrylic polyoxy second is added into reaction vessel Alkene ether, during to methyl allyl polyoxyethylene ether stirring and dissolving more than 90%, input acrylic acid is stirred 10-15 minutes, and third is added afterwards Acrylamide is stirred 2 minutes;

Step 2: adding hydrogen peroxide in the reaction vessel of step one, crossing ammonium, and stir 3-5 minutes, start that A material and B is added dropwise Material;A material parts by weights includes 8-16 parts of acrylic acid, 30-60 parts of hydroxy-ethyl acrylate, 20-30 parts of hydrogen peroxide;B expects parts by weights Including 50-90 parts of hydrogen peroxide;

Step 3: control reaction vessel interior temperature is between 10-35 DEG C, A gobs add 2.5-3.0 hours, and B gobs add 3.0- 3.5 hours, it is incubated 1.5 hours, you can obtained to protect the sustained-release polycarboxylic water reducer that collapses.

It is preferred that, in step 2, A material parts by weights includes 12 parts of acrylic acid, 40 parts of hydroxy-ethyl acrylate, hydrogen peroxide 24 Part;B material parts by weights includes 60 parts of hydrogen peroxide.

It is preferred that, in step 2, A material parts by weights includes 14 parts of acrylic acid, 50 parts of hydroxy-ethyl acrylate, hydrogen peroxide 26 Part;B material parts by weights includes 70 parts of hydrogen peroxide.

One kind proposed by the present invention protects the sustained-release polycarboxylic water reducer normal temperature synthesis technique that collapses, and the sustained release that collapses is protected relative to tradition Type polycarboxylate water-reducer manufacturing process, preparation method is simple, easy to operate, to protect a large amount of lifes for the sustained-release polycarboxylic water reducer that collapses Production provides road.

Embodiment

With reference to specific embodiment, the present invention will be further described.

Embodiment one

One kind protects the sustained-release polycarboxylic water reducer normal temperature synthesis technique that collapses, and comprises the following steps:

Step 1: adding bottom water, 10 DEG C of water temperature in reaction vessel;Methacrylic polyoxyethylene is added into reaction vessel Ether, during to methyl allyl polyoxyethylene ether stirring and dissolving more than 90%, input acrylic acid is stirred 10 minutes, and acryloyl is added afterwards Amine is stirred 2 minutes;

Step 2: adding hydrogen peroxide in the reaction vessel of step one, crossing ammonium, and stir 3 minutes, start that A material and B material is added dropwise;A Expect that parts by weights includes 8 parts of acrylic acid, 31 parts of hydroxy-ethyl acrylate, 21 parts of hydrogen peroxide;B material parts by weights includes hydrogen peroxide 51 Part;

Step 3: control reaction vessel interior temperature is at 10 DEG C, A gobs add 2.5 hours, and B gobs add 3.0 hours, and insulation 1.5 is small When, you can obtained guarantor is collapsed sustained-release polycarboxylic water reducer.

Embodiment two

One kind protects the sustained-release polycarboxylic water reducer normal temperature synthesis technique that collapses, and comprises the following steps:

Step 1: adding bottom water, 15 DEG C of water temperature in reaction vessel;Methacrylic polyoxyethylene is added into reaction vessel Ether, during to methyl allyl polyoxyethylene ether stirring and dissolving more than 90%, input acrylic acid is stirred 12 minutes, and acryloyl is added afterwards Amine is stirred 2 minutes;

Step 2: adding hydrogen peroxide in the reaction vessel of step one, crossing ammonium, and stir 4 minutes, start that A material and B material is added dropwise;A Expect that parts by weights includes 12 parts of acrylic acid, 40 parts of hydroxy-ethyl acrylate, 24 parts of hydrogen peroxide;B material parts by weights includes hydrogen peroxide 60 Part;

Step 3: control reaction vessel interior temperature is at 15 DEG C, A gobs add 2.7 hours, and B gobs add 3.2 hours, and insulation 1.5 is small When, you can obtained guarantor is collapsed sustained-release polycarboxylic water reducer.

Embodiment three

One kind protects the sustained-release polycarboxylic water reducer normal temperature synthesis technique that collapses, and comprises the following steps:

Step 1: adding bottom water, 25 DEG C of water temperature in reaction vessel;Methacrylic polyoxyethylene is added into reaction vessel Ether, during to methyl allyl polyoxyethylene ether stirring and dissolving more than 90%, input acrylic acid is stirred 13 minutes, and acryloyl is added afterwards Amine is stirred 2 minutes;

Step 2: adding hydrogen peroxide in the reaction vessel of step one, crossing ammonium, and stir 4 minutes, start that A material and B material is added dropwise;A Expect that parts by weights includes 14 parts of acrylic acid, 50 parts of hydroxy-ethyl acrylate, 26 parts of hydrogen peroxide;B material parts by weights includes hydrogen peroxide 70 Part;

Step 3: control reaction vessel interior temperature is at 30 DEG C, A gobs add 2.8 hours, and B gobs add 3.4 hours, and insulation 1.5 is small When, you can obtained guarantor is collapsed sustained-release polycarboxylic water reducer.

Example IV

One kind protects the sustained-release polycarboxylic water reducer normal temperature synthesis technique that collapses, and comprises the following steps:

Step 1: adding bottom water, 35 DEG C of water temperature in reaction vessel;Methacrylic polyoxyethylene is added into reaction vessel Ether, during to methyl allyl polyoxyethylene ether stirring and dissolving more than 90%, input acrylic acid is stirred 15 minutes, and acryloyl is added afterwards Amine is stirred 2 minutes;

Step 2: adding hydrogen peroxide in the reaction vessel of step one, crossing ammonium, and stir 5 minutes, start that A material and B material is added dropwise;A Expect that parts by weights includes 16 parts of acrylic acid, 60 parts of hydroxy-ethyl acrylate, 30 parts of hydrogen peroxide;B material parts by weights includes hydrogen peroxide 90 Part;

Step 3: control reaction vessel interior temperature is at 35 DEG C, A gobs add 3.0 hours, and B gobs add 3.5 hours, and insulation 1.5 is small When, you can obtained guarantor is collapsed sustained-release polycarboxylic water reducer.

The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto, it is any Those familiar with the art the invention discloses technical scope in, technique according to the invention scheme and its invention Design is subject to equivalent substitution or change, should all be included within the scope of the present invention.

Claims (3)

1. one kind protects the sustained-release polycarboxylic water reducer normal temperature synthesis technique that collapses, it is characterised in that comprise the following steps:
Step 1: adding bottom water, 10-35 DEG C of water temperature in reaction vessel;Methacrylic polyoxy second is added into reaction vessel Alkene ether, during to methyl allyl polyoxyethylene ether stirring and dissolving more than 90%, input acrylic acid is stirred 10-15 minutes, and third is added afterwards Acrylamide is stirred 2 minutes;
Step 2: adding hydrogen peroxide in the reaction vessel of step one, crossing ammonium, and stir 3-5 minutes, start that A material and B is added dropwise Material;A material parts by weights includes 8-16 parts of acrylic acid, 30-60 parts of hydroxy-ethyl acrylate, 20-30 parts of hydrogen peroxide;B expects parts by weights Including 50-90 parts of hydrogen peroxide;
Step 3: control reaction vessel interior temperature is between 10-35 DEG C, A gobs add 2.5-3.0 hours, and B gobs add 3.0- 3.5 hours, it is incubated 1.5 hours, you can obtained to protect the sustained-release polycarboxylic water reducer that collapses.
The sustained-release polycarboxylic water reducer normal temperature synthesis technique 2. a kind of guarantor according to claim 1 is collapsed, it is characterised in that In step 2, A material parts by weights includes 12 parts of acrylic acid, 40 parts of hydroxy-ethyl acrylate, 24 parts of hydrogen peroxide;B expects subpackage by weight Include 60 parts of hydrogen peroxide.
The sustained-release polycarboxylic water reducer normal temperature synthesis technique 3. a kind of guarantor according to claim 1 is collapsed, it is characterised in that In step 2, A material parts by weights includes 14 parts of acrylic acid, 50 parts of hydroxy-ethyl acrylate, 26 parts of hydrogen peroxide;B expects subpackage by weight Include 70 parts of hydrogen peroxide.
CN201710575903.6A 2017-07-14 2017-07-14 One kind protects the sustained-release polycarboxylic water reducer normal temperature synthesis technique that collapses CN107325235A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102504126A (en) * 2011-11-03 2012-06-20 山西合盛邦砼建材有限公司 Slump loss resistant type gather carboxylate water-reducing agent and preparation method thereof
CN103172291A (en) * 2012-12-14 2013-06-26 上海东大化学有限公司 Polycarboxylic-acid water reducing agent synthesized at normal temperature, and preparation method and application method thereof
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
CN104371076A (en) * 2014-12-04 2015-02-25 河北铁园科技发展有限公司 Method of synthesizing polycarboxylate superplasticizer at normal temperature
CN105110687A (en) * 2015-07-30 2015-12-02 厦门路桥翔通建材科技有限公司 Mud resisting and slump retaining type polycarboxylic acids water reducer and preparation method thereof
CN105542092A (en) * 2016-01-20 2016-05-04 南京师范大学 Method for synthesizing slow release type high slump loss resistant polycarboxylate water reducer at normal temperature

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102504126A (en) * 2011-11-03 2012-06-20 山西合盛邦砼建材有限公司 Slump loss resistant type gather carboxylate water-reducing agent and preparation method thereof
CN103172291A (en) * 2012-12-14 2013-06-26 上海东大化学有限公司 Polycarboxylic-acid water reducing agent synthesized at normal temperature, and preparation method and application method thereof
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
CN104371076A (en) * 2014-12-04 2015-02-25 河北铁园科技发展有限公司 Method of synthesizing polycarboxylate superplasticizer at normal temperature
CN105110687A (en) * 2015-07-30 2015-12-02 厦门路桥翔通建材科技有限公司 Mud resisting and slump retaining type polycarboxylic acids water reducer and preparation method thereof
CN105542092A (en) * 2016-01-20 2016-05-04 南京师范大学 Method for synthesizing slow release type high slump loss resistant polycarboxylate water reducer at normal temperature

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