CN114853809A - Preparation method and application of water-soluble functional aid 3-chloro-2-hydroxy sodium propanephosphonate - Google Patents
Preparation method and application of water-soluble functional aid 3-chloro-2-hydroxy sodium propanephosphonate Download PDFInfo
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- CN114853809A CN114853809A CN202210434575.9A CN202210434575A CN114853809A CN 114853809 A CN114853809 A CN 114853809A CN 202210434575 A CN202210434575 A CN 202210434575A CN 114853809 A CN114853809 A CN 114853809A
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- water
- chloro
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- sodium
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/38—Phosphonic acids RP(=O)(OH)2; Thiophosphonic acids, i.e. RP(=X)(XH)2 (X = S, Se)
- C07F9/3804—Phosphonic acids RP(=O)(OH)2; Thiophosphonic acids, i.e. RP(=X)(XH)2 (X = S, Se) not used, see subgroups
- C07F9/3808—Acyclic saturated acids which can have further substituents on alkyl
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/005—Halogen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
The invention discloses a preparation method and application of a water-soluble functional aid 3 chloro 2 sodium hydroxy propyl phosphonate, wherein water and phosphorous acid are added into a reaction kettle to be heated to 80-85 ℃, then epichlorohydrin is dripped, the temperature is controlled not to exceed 85 ℃, the reaction is continued, and a product is separated to obtain the 3 chloro 2 sodium hydroxy propyl phosphonate. The product is a water-soluble functional monomer, can be grafted on the concrete polycarboxylate superplasticizer molecule, greatly reduces the sensitivity of the polycarboxylate superplasticizer to materials and the large loss of concrete slump caused by the deterioration of raw materials, modifies the polycarboxylate superplasticizer, changes the defects of the original polycarboxylate superplasticizer in concrete application, improves the working performance of concrete, can also be used for modifying a water treatment agent, and increases the dispersion performance of the original water treatment agent.
Description
Technical Field
The invention relates to the technical field of organic chemistry, in particular to a preparation method and application of a water-soluble functional assistant 3 chloro 2 hydroxy sodium propanephosphonate.
Background
With the acceleration of the urbanization speed in China, various mortar products including self-leveling mortar, tile glue, grouting material and the like are increasingly widely used in civilian use and industry, so that higher requirements are put forward on the performance of the mortar. The water reducing agent is used as one of mortar additives and is applied to dry powder mortar in a large amount, the traditional mortar water reducing agent mainly comprises naphthalene and polyamines, and the conventional powder polycarboxylate water reducing agent greatly improves the fluidity, the construction property, the strength and the like of the mortar when being applied to mortar products due to the higher water reducing rate and the good fluidity retentivity of the existing powder polycarboxylate water reducing agent.
However, the technology of the polycarboxylate superplasticizer is not mature, the polycarboxylate superplasticizer in the prior art has many defects, and the applied concrete has poor performance, various defects are caused, and the actual construction requirements are difficult to meet.
Therefore, how to provide a novel high-performance polycarboxylate superplasticizer modifier is a problem to be solved urgently by those skilled in the art.
Disclosure of Invention
In view of the above, the invention provides a preparation method and application of a water-soluble functional assistant, namely sodium 3 chloro-2 hydroxypropionate.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of water-soluble functional aid 3 chloro 2 sodium hydroxypropionate comprises the following processes:
adding water and phosphorous acid into a reaction kettle, heating to 80-85 ℃, then dropwise adding epoxy chloropropane, controlling the temperature not to exceed 85 ℃, continuously reacting for 2h, and separating a product to obtain the 3-chloro-2-hydroxy sodium propanephosphonate.
Preferably, the mass ratio of water: phosphorous acid: epichlorohydrin 8:42: 47.
The invention also provides application of the water-soluble functional auxiliary agent 3-chloro-2-hydroxy sodium propanephosphonate in preparation of a modified polycarboxylic acid water reducing agent.
The preparation method of the modified polycarboxylate superplasticizer comprises the following steps:
and (2) putting the 3-chloro-2-hydroxy sodium propanephosphonate in a reaction kettle, heating to 50 ℃, dropwise adding a polyether monomer, acrylic acid and a catalyst VC, and reacting to obtain the modified polycarboxylic acid water reducer.
Preferably, the mass ratio of 3 chloro 2 sodium hydroxypropionate: polyether monomer: acrylic acid: catalyst VC ═ 20: 350:45:0.6.
Preferably, the polyether monomer is methyl allyl polyoxyethylene ether.
The invention also provides application of the water-soluble functional auxiliary agent 3-chloro-2-hydroxy sodium propanephosphonate in preparation of modified water treatment agents.
The preparation method of the modified water treatment agent comprises the following steps:
and dropwise adding 3-chloro-2-hydroxy sodium propanephosphonate into polyepoxysuccinic acid to react for 4 hours, controlling the reaction temperature to be less than or equal to 35 ℃, and cooling after the reaction is finished to obtain the modified water treatment agent.
Preferably, the mass ratio of 3 chloro 2 sodium hydroxypropionate: polyepoxysuccinic acid ═ 1: 2.
According to the technical scheme, compared with the prior art, the invention discloses a preparation method of a water-soluble functional auxiliary agent 3 chloro 2 hydroxy sodium propanephosphonate, which has the following beneficial effects: the product is a water-soluble functional monomer, can be grafted on the concrete polycarboxylate superplasticizer molecule, greatly reduces the sensitivity of the polycarboxylate superplasticizer to materials and the large loss of concrete slump caused by the deterioration of raw materials, modifies the polycarboxylate superplasticizer, changes the defects of the original polycarboxylate superplasticizer in concrete application, improves the working performance of concrete, can also be used for modifying a water treatment agent, and increases the dispersion performance of the original water treatment agent.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
preparation of water-soluble functional assistant 3 chloro-2-hydroxy sodium propanephosphonate:
adding 40g of water and 210g of phosphorous acid into a reaction kettle, heating to 80-85 ℃, then dropwise adding 235g of epichlorohydrin, controlling the temperature not to exceed 85 ℃, continuously reacting for 2h, and separating a product to obtain the 3-chloro-2-hydroxypropiophosphate sodium.
Example 2:
preparing a modified polycarboxylic acid water reducing agent:
20Kg of sodium 3-chloro-2-hydroxypropionate is placed in a reaction kettle, heated to 50 ℃, and added with 350Kg of polyether monomer (methyl allyl polyoxyethylene ether), 45Kg of acrylic acid and VC0.6Kg of catalyst dropwise to react to prepare the modified polycarboxylic acid water reducer.
Example 3:
preparing a modified water treatment agent:
and (3) dropwise adding 10g of sodium 3-chloro-2-hydroxypropionate into 20g of polyepoxysuccinic acid to react for 4 hours, controlling the reaction temperature to be less than or equal to 35 ℃, and cooling after the reaction is finished to obtain the modified water treatment agent.
Test example:
comparison of Experimental results of modified Water reducing agent
Modified water treatment agent
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed in the embodiment corresponds to the method disclosed in the embodiment, so that the description is simple, and the relevant points can be referred to the description of the method part.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A preparation method of a water-soluble functional assistant 3 chloro 2 hydroxy sodium propanephosphonate is characterized by comprising the following processes:
adding water and phosphorous acid into a reaction kettle, heating to 80-85 ℃, then dropwise adding epoxy chloropropane, controlling the temperature not to exceed 85 ℃, continuously reacting for 2h, and separating a product to obtain the 3-chloro-2-hydroxy sodium propanephosphonate.
2. The preparation method of the water-soluble functional assistant sodium 3 chloro-2 hydroxypropionate according to claim 1, characterized in that the mass ratio of water: phosphorous acid: epichlorohydrin 8:42: 47.
3. The application of the water-soluble functional assistant sodium 3 chloro-2 hydroxypropionate in claim 1 in the preparation of modified polycarboxylate superplasticizer.
4. The preparation method of the modified polycarboxylate water reducer of claim 3 is characterized by comprising the following steps:
and (2) putting the 3-chloro-2-hydroxy sodium propanephosphonate in a reaction kettle, heating to 50 ℃, dropwise adding a polyether monomer, acrylic acid and a catalyst VC, and reacting to obtain the modified polycarboxylic acid water reducer.
5. The preparation method of the modified polycarboxylate water reducer according to claim 4, characterized in that the mass ratio of the sodium 3-chloro-2-hydroxypropionate: polyether monomer: acrylic acid: catalyst VC is 20:350:45: 0.6.
6. The preparation method of the modified polycarboxylate water reducer as claimed in claim 4 or 5, wherein the polyether monomer is methyl allyl polyoxyethylene ether.
7. The application of the water-soluble functional assistant 3-chloro-2-hydroxypropionic acid sodium salt in claim 1 in preparation of modified water treatment agents.
8. The method for preparing a modified water treatment agent according to claim 7, comprising the steps of:
and dropwise adding 3-chloro-2-hydroxy sodium propanephosphonate into polyepoxysuccinic acid to react for 4 hours, controlling the reaction temperature to be less than or equal to 35 ℃, and cooling after the reaction is finished to obtain the modified water treatment agent.
9. The method for preparing a modified water treatment agent according to claim 9, wherein the ratio by mass of sodium 3 chloro-2 hydroxypropionate: polyepoxysuccinic acid ═ 1: 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210434575.9A CN114853809A (en) | 2022-04-24 | 2022-04-24 | Preparation method and application of water-soluble functional aid 3-chloro-2-hydroxy sodium propanephosphonate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210434575.9A CN114853809A (en) | 2022-04-24 | 2022-04-24 | Preparation method and application of water-soluble functional aid 3-chloro-2-hydroxy sodium propanephosphonate |
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| CN114853809A true CN114853809A (en) | 2022-08-05 |
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| CN202210434575.9A Pending CN114853809A (en) | 2022-04-24 | 2022-04-24 | Preparation method and application of water-soluble functional aid 3-chloro-2-hydroxy sodium propanephosphonate |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6451775B1 (en) * | 2001-08-29 | 2002-09-17 | Colonial Chemical Inc. | Castor amidopropyl dimethyl phospholipids as emulsifiers |
| US6620794B1 (en) * | 2002-07-08 | 2003-09-16 | Colonial Chemical Inc. | Guerbet functionalized phospholipids |
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2022
- 2022-04-24 CN CN202210434575.9A patent/CN114853809A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6451775B1 (en) * | 2001-08-29 | 2002-09-17 | Colonial Chemical Inc. | Castor amidopropyl dimethyl phospholipids as emulsifiers |
| US6620794B1 (en) * | 2002-07-08 | 2003-09-16 | Colonial Chemical Inc. | Guerbet functionalized phospholipids |
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