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Method for preparing polyether for polycarboxylic acid series concrete additive

A technology for concrete admixtures and polycarboxylates, which is applied in the field of preparation of polyethers for polycarboxylate concrete admixtures, and can solve the problem of increasing the synthesis process route of polycarboxylate concrete admixtures, reducing the quality of raw materials, and polyether molecules. Short chain and other problems, to achieve the effect of superior product quality, improved quality, and narrow molecular weight distribution

Active Publication Date: 2008-04-23
NANJING BOTE BUILDING MATERIALS CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The technical problem to be solved by the present invention is the following deficiencies in the existing polycarboxylate concrete admixture polyether raw material or its production equipment: 1. the polyether molecular chain is relatively too short, and the molecular weight distribution is too wide; 2. most of the production equipment In addition to causing a high content of residual raw material oxyalkylene (mainly referring to ethylene oxide, propylene oxide, or a mixture of ethylene oxide and propylene oxide) in the product, it is also prone to explosion, poisoning or environmental pollution; ③ the prepared single Alkyl polyethers need to be esterified to prepare functional monomers with polymerization activity before they can be used to synthesize polycarboxylate concrete admixtures. This not only increases the synthesis process route of polycarboxylate concrete admixtures, but also causes On the one hand, the degree of esterification cannot reach 100%, resulting in a reduction in the quality of the raw materials for the synthesis of polycarboxylic acid-based concrete admixtures; It is a substance with serious hazards in the process of concrete admixture; ④ Although it has been reported that unsaturated monomers (such as allyl alcohol, hydroxyethyl acrylate, hydroxypropyl acrylate, etc.) were used as an alkoxylation initiator to prepare in one step Process with polymerizable living polyethers, but limited to continuous stirred tank reactors

Method used

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  • Method for preparing polyether for polycarboxylic acid series concrete additive
  • Method for preparing polyether for polycarboxylic acid series concrete additive
  • Method for preparing polyether for polycarboxylic acid series concrete additive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Replace the whole set of equipment with nitrogen (N2), add 3193.30kg hydroxyethyl acrylate, 18.83kgNaOH and 31.93kg1, 4-naphthoquinone to the loop reactor pre-reactor (R-2202), vacuumize (-750mmHg) and heat up to 100 Dehydrate at ℃ for 50 minutes, fill the pre-reactor with N2 to make the pressure of the pre-reactor reach 0.3Mpa, start the small circulation pump (P-2214), and press in 20.71kg of ethylene oxide at the same time to start the reaction for 2 hours; then turn on the large circulation pump (P-2204), press Add ethylene oxide into the reactor at a rate of 3762.70kg / h, polymerize at 160°C and a pressure of 0.3Mpa, maintain the feeding and reaction for 5h, stop adding ethylene oxide, and continue to circulate and mature for 5min; When the pressure no longer decreases, the reaction is over, and the vacuum is turned on to remove free ethylene oxide in the reactor and passed into the polyether tail gas treatment tower for water washing treatment, and the tail gas is d...

Embodiment 2

[0041] Replace the whole set of equipment with nitrogen (N2), add 2863.08kg hydroxyethyl methacrylate, 14.37kgNaOH and 13.32kg1, 4-benzoquinone to the loop reactor pre-reactor (R-2202), vacuumize (-750mmHg) to raise the temperature Dehydrate at 100°C for 50 minutes, fill the pre-reactor with N2 to make the pressure of the pre-reactor reach 0.3Mpa, start the small circulation pump (P-2214), and press 15.81kg of ethylene oxide at the same time to start the reaction for 2 hours; then turn on the large circulation pump (P-2204) , add ethylene oxide to the reactor at a rate of 3190.52kg / h, polymerize at 160°C and a pressure of 0.3Mpa, keep feeding and reacting for 6 hours, stop adding ethylene oxide, and continue to circulate for 7 minutes; when the reaction When the pressure in the reactor no longer decreases, the reaction is over, and the vacuum is turned on to remove the free ethylene oxide in the reactor and passed into the polyether tail gas treatment tower for water washing tr...

Embodiment 3

[0043] Replace the whole set of equipment with nitrogen (N2), add 1431.54kg hydroxypropyl acrylate, 10.29kgNaOH and 3.58kg1, 4-benzoquinone to the loop reactor pre-reactor (R-2202), vacuumize (-750mmHg) and raise the temperature to 100 Dehydrate at ℃ for 50 minutes, fill the pre-reactor with N2 to make the pressure of the pre-reactor reach 0.3Mpa, start the small circulation pump (P-2214), and press in 11.32kg of ethylene oxide at the same time to start the reaction for 2 hours; then turn on the large circulation pump (P-2204), press Add oxyalkylene into the reactor at a rate of 2938.30kg / h, polymerize at 160°C and a pressure of 0.3Mpa, maintain the feeding and reaction for 7h, stop adding ethylene oxide, and continue to circulate and mature for 8min; When it decreases again, the reaction ends, and the vacuum is opened to remove free ethylene oxide in the reactor and passed into the polyether tail gas treatment tower for water washing treatment, and the tail gas is discharged i...

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Abstract

This invention relates to a method for preparing polyether used specially for the production of poly-carboxylic acid series concrete additive. In this invention method, (1), X-O-H is used as the initiator for the oxyalkylene ring-opening polymerization to prepare polymerizable active polyether; where in the 'X' represents the group as it is in the formula (1); (2), the above-mentioned polyether is used for BUSS alkoxylation. This invention has advantages of: (1)the molecular weight of the polyether can be controlled by 190-4000, narrow molecular weight distribution, flexible operation, excellent quality of product; (2)no procedure of esterification in this inventive production; (3)safety production, no need of solvent; (4)large scale batch production.

Description

technical field [0001] The invention relates to a preparation method of a special polyether for a concrete admixture, in particular to a preparation method of a special polyether for a polycarboxylate concrete admixture. Background technique [0002] Concrete superplasticizer (high-efficiency water reducer) especially high-performance admixture is the most effective, simple and economical way to reduce the amount of cement, increase the utilization rate of industrial waste residue, increase the strength level of concrete and improve the durability of concrete. The indispensable fifth component of high-performance and durable concrete is also the most important basic material for the concrete industry to achieve sustainable development strategies. However, traditional polycondensation-type admixtures such as naphthalene-based and melamine-based admixtures have problems such as low water-reducing rate, large slump loss, and increased shrinkage, and the production process pollu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B24/32C08G71/02
Inventor 刘加平缪昌文张月星冉千平陈宋辉游有鲲
Owner NANJING BOTE BUILDING MATERIALS CO LTD
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