Preparation method of polycarboxylic acid water reducing agent containing phosphate group

A technology of phosphonic acid-based and water-reducers, which is applied in the field of preparation of polycarboxylate water-reducers, and can solve the problems of being unsuitable for industrial production, the monomer yield cannot be effectively guaranteed, and the preparation method is complicated.

A technology of phosphonic acid-based and water-reducers, which is applied in the field of preparation of polycarboxylate water-reducers, and can solve the problems of being unsuitable for industrial production, the monomer yield cannot be effectively guaranteed, and the preparation method is complicated.

CN106832147AActive Publication Date: 2017-06-13山西科腾环保新材料股份有限公司
8 Cites 16 Cited by

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of polycarboxylic acid water reducing agent containing phosphate group
  • Preparation method of polycarboxylic acid water reducing agent containing phosphate group
  • Preparation method of polycarboxylic acid water reducing agent containing phosphate group

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The first step is to prepare terminal ethylenically unsaturated phosphonic acid monomer: the molar ratio of phosphorous acid, acrylic acid, acryloyl chloride and water is 1:2:1.1:1. In the tube, thermometer, dropping funnel, and cold water bath flask, first add the calculated phosphorous acid according to the proportion, then add the calculated acrylic acid and a small amount of polymerization inhibitor, and then drop the calculated amount of acryloyl chloride and keep stirring. The dropping time is about 1h, the temperature of the water bath is controlled below 60~65°C. After the addition, continue to stir and react at this temperature for 30min; then slowly raise the temperature to 110~120°C, stir and reflux for 2h to absorb the hydrogen chloride gas generated; after the reaction, Add the calculated amount of water and distill under reduced pressure for 1~2 hours to remove acrylic acid and residual HCl gas. After the reaction is completed, hydroxypropenylidene diphosph...

Embodiment 2

[0032] The preparation process of terminal alkenyl phosphonic acid monomer is exactly the same as that of Example 1. Methallyl polyoxyethylene ether (molecular weight 2400), acrylic acid and unsaturated phosphonic acid are measured in a molar ratio of 1.0: 3.36: 0.84, and acrylic acid, unsaturated phosphonic acid monomer, deionized Water and chain transfer agent are mixed to obtain liquid A for dropwise addition. Other conditions are exactly the same as in Example 1, and the mother liquid of polycarboxylate superplasticizer can be prepared, which is marked as PC2. See the experimental data Table 1 and Table 2 for the experimental data.

Embodiment 3

[0034] The raw material ratio of terminal alkenyl phosphonic acid monomer preparation process is that the molar ratio of phosphorous acid, acrylic acid, methacryloyl chloride and water is 1:2.5:1.1:1, and the other processes and other process conditions are exactly the same as in Example 1, and the obtained The product is hydroxymethylacrylidene diphosphonic acid. The product is dubbed into a 40% solution after analysis. The three monomers of methallyl polyoxyethylene ether (molecular weight 2400), acrylic acid, and the above-mentioned ethylenically unsaturated phosphonic acid are measured in a molar ratio of 1.0: 3.5: 0.7, and the acrylic acid, unsaturated phosphonic acid mono Body, deionized water and chain transfer agent are mixed to obtain liquid A for dropwise addition of reaction; other conditions are exactly the same as in Example 1, and the mother liquid of polycarboxylate superplasticizer can be prepared, which is marked as PC3. See the experimental data Table 1 and ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention provides a preparation method of a polycarboxylic acid water reducing agent containing a phosphate group. The preparation method comprises the following steps: firstly, preparing a terminal alkenyl unsaturated phosphonic acid monomer; secondly, mixing acrylic acid, the unsaturated phosphonic acid monomer, a chain transferring agent and de-ionized water to prepare a mixed monomer solution; by taking an alkenyl polyoxyethylene ether macro-monomer solution as a base material, dropwise adding an initiator water solution and the mixed monomer solution respectively under a room-temperature polymerization condition; uniformly stirring, dropwise adding and reacting; and finally neutralizing with a sodium hydroxide solution to obtain the polycarboxylic acid water reducing agent. According to the water reducing agent, the terminal alkenyl unsaturated phosphonic acid monomer is introduced into a structure and primary adsorption is facilitated; the initial dispersity is improved, and hydration and agglomeration of cement are delayed; the slump retaining property is effectively improved and the sensitivity to concrete is reduced; and the stress resistance and adaptability on different aggregate are enhanced.

Description

technical field [0001] The present invention relates to a preparation method of polycarboxylate water-reducer containing phosphonic acid groups, especially the polycarboxylate water-reducer which introduces terminal ethylenically unsaturated phosphonic acid as polymerized monomer into the structure of traditional water reducer Preparation. [0002] Background of the invention [0003] Under the condition of low water-cement ratio and low dosage, polycarboxylate superplasticizer has the outstanding advantages of high pulp fluidity, small slump loss, and environmental protection. Due to the gradual deterioration of sand and gravel resources all over the country during the mixing process of concrete, polycarboxylate superplasticizers are very sensitive to the minerals in clay compared to cement. Therefore, polycarboxylate superplasticizers have a strong tendency to adsorb clay, which has a great impact on the transportation, retention and strength of concrete during constructio...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
13 Jun 2017
Publication
CN106832147A
IPC
C08F283/06; C08F220/06; C08F230/02; C08F4/40; C04B24/24; C04B103/30
CPC
C04B24/246; C04B2103/302; C08F4/40; C08F283/065; C08F220/06; C08F230/02
Inventors
吕志平; 范向前