Preparation method of polycarboxylate water reducer containing polyether side chains

A technology of polyether side chain and polycarboxylic acid, which is applied in the field of preparation of polycarboxylate water reducer, can solve the influence of polycarboxylate water reducer on performance, reduce the molecular weight of polycarboxylate water reducer, and reduce the double bond content To achieve the effect of good concrete application performance, mild conditions and simple process

Inactive Publication Date: 2015-06-10
LIAONING OXIRANCHEM INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, compared with the liquid polycarboxylate water reducer, the solid polycarboxylate water reducer currently on the market has a large gap in application performance, so the solid polycarboxylate water reducer has not yet completely replaced the liquid polycarboxylate water reducer. Liquid
[0004] The polycarboxylate water reducer containing polyether side chains is a common high-efficiency polycarboxylate water reducer. The conventional preparation process is to copolymerize macromonomers containing polyether chains and unsaturated carboxylic acid monomers. (such as Chinese patent CN 102140018A, etc.), in this preparation method, due to the high temperature in the production process of the polyether chain-containing macromonomer, the double bond component with polymerization activity in the monomer is greatly damaged, and its double bond The bond retention rate is only about 90%, which reduces the double bond content when participating in the synthesis of the water reducer, and reduces the molecular weight of the polycarboxylate water reducer, so that the obtained polycarboxylate water reducer product is also affected in terms of performance. affected

Method used

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  • Preparation method of polycarboxylate water reducer containing polyether side chains
  • Preparation method of polycarboxylate water reducer containing polyether side chains
  • Preparation method of polycarboxylate water reducer containing polyether side chains

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Add 10.05g of 2-methallyl alcohol, 80g of dimethyl sulfoxide, 1.35g of hydrogen peroxide, 40g of acrylic acid, 1.2g of mercaptoacetic acid and 0.4g of vitamin C into the reaction kettle, at 60±5℃ Under full stirring, reacted for 3.5 hours.

[0042] Add sodium hydride to neutralize the polymer product to pH=6~8. Continue to add 0.2g of sodium hydroxide, and raise the temperature to 120°C, continue to add 325g of ethylene oxide, and keep the reaction temperature between 120 and 180°C. After the reaction is completely stopped, add acetic acid to neutralize the sodium hydroxide.

[0043] The obtained product is spray-dried to obtain a solid powdery polycarboxylate water reducer product.

[0044] The obtained polycarboxylate water reducer product is made into an aqueous solution with a mass concentration of 20%, and the measured viscosity is 11.32mm according to the kinematic viscosity measurement method of GB / T265-88 petroleum products. 2 / s.

Embodiment 2

[0046] Add 8.1g of allyl alcohol, 100g of N,N-dimethylformamide, 1.35g of hydrogen peroxide, 54.4g of maleic anhydride, 1.2g of thioglycolic acid and 0.4g of vitamin C into the reaction kettle together, at 50±5 Under the condition of ℃, fully stir and react for 4 hours.

[0047]Add metal sodium to neutralize the polymer product to pH=6~8. Continue to add 0.2 g of sodium hydroxide, raise the temperature to 120° C., and continuously add 327 g of ethylene oxide. Keep the reaction temperature between 120 and 180°C, and add phosphoric acid to neutralize after the reaction is completely stopped.

[0048] The obtained product is spray-dried to obtain a solid powdery polycarboxylate water reducer product.

[0049] The obtained polycarboxylate water reducer product is made into an aqueous solution with a mass concentration of 20%, and the measured viscosity is 8.12mm according to the kinematic viscosity measurement method of GB / T265-88 petroleum products. 2 / s.

Embodiment 3

[0051] 12g of 3-methyl-3-buten-1-alcohol, 120g dimethyl sulfoxide, 1.35g hydrogen peroxide, 40g acrylic acid, 1.2g thioglycolic acid and 0.4g vitamin C were added to the reactor together, Stir well at 65±5°C and react for 5 hours.

[0052] Add potassium hydride to neutralize the polymer product to pH=6~8. Continue to add 0.2 g of sodium hydroxide, raise the temperature to 120° C., and continuously add 323 g of ethylene oxide. Keep the reaction temperature between 120 and 180°C, and add acetic acid to neutralize after the reaction is completely stopped.

[0053] The obtained product is spray-dried to obtain a solid powdery polycarboxylate water reducer product.

[0054] The obtained polycarboxylate water reducer product is made into an aqueous solution with a mass concentration of 20%, and the measured viscosity is 12.44mm according to the kinematic viscosity measurement method of GB / T265-88 petroleum products 2 / s. .

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Abstract

The invention provides a preparation method of a polycarboxylate water reducer containing polyether side chains. The preparation method comprises the following steps: firstly, carrying out copolymerization on terminal alkenyl-containing alcohol and unsaturated carboxylic acid or anhydride to prepare a copolymer; and then carrying out oxyalkylation reaction on the obtained copolymer and epoxyalkane to obtain the polycarboxylate water reducer. The preparation method provided by the invention firstly prepares a main chain structure of the polycarboxylate water reducer through copolymerization and then forms the polyether side chains through oxyalkylation reaction. As the double bonds of a polymer monomer forming the main chain structure are not damaged, the double bond retention rate of the monomer is high, the polymerization effect is relatively good, and the viscosity of the obtained polycarboxylate water reducer is relatively high. The polycarboxylate water reducer prepared by the preparation method is obviously superior to that of a product prepared by the existing preparation method in concrete application performance. The preparation method provided by the invention is simple and convenient in process, mild in condition and strong in operability.

Description

technical field [0001] The invention relates to the field of high molecular polymers, in particular to a preparation method of a polycarboxylate water reducer containing polyether side chains. Background technique [0002] Polycarboxylate superplasticizer is a new type of concrete additive. It not only has a high concrete water reducing rate and good concrete fluidity, but the most important thing is that the fresh concrete mixed with polycarboxylate superplasticizer slumps The slump loss is small, the strength of the formed concrete is higher, the later drying shrinkage of the concrete is relatively small, and it has superior performance in various aspects such as corrosion resistance and aging resistance. At the same time, in the production process of polycarboxylate superplasticizer, its molecular structure has strong designability, and its molecular weight, molecular structure, type and arrangement of functional groups can be adjusted according to needs. The production p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C08F216/04C08F216/08C08F222/02C08F220/06C08F222/06C08F2/38C04B24/32C04B103/30
Inventor 朱建民刘兆滨董振鹏周立明张楠
Owner LIAONING OXIRANCHEM INC
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