Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of block-type high polymerization degree macromonomer methyl allyl polyoxyethylene polyoxypropylene ether

A technology of methyl alkenyl polyoxyethylene polyoxypropylene ether and high degree of polymerization, which is applied in the field of polyether synthesis in organic chemistry, and can solve the problem that the performance cannot meet the polymerization requirements of polycarboxylate water reducers, the molecular weight is difficult to increase, and the molecular weight Wide distribution and other issues, to achieve the effect of improving the double bond retention rate, high degree of polymerization, and high reactivity

Active Publication Date: 2014-05-07
XINGTAI LANTIAN FINE CHEM
View PDF6 Cites 11 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the reactive structural characteristics of the methyl alkenyl alcohol polyether macromonomer and the trace moisture in the raw materials that are not easily removed during production, PEG is easy to form; the macromonomer is also prone to rearrangement reactions during synthesis, resulting in "internal "ene" and other impurities; in the production of block and random polyether, the chain transfer rearrangement reaction of propylene oxide also causes low molecular weight and wide molecular weight distribution
These factors make it difficult to increase the molecular weight and high impurity content in the synthesis of high-polymerization polyether macromonomers, resulting in its performance not meeting the polymerization requirements of polycarboxylate superplasticizers.

Method used

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
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of block-type high polymerization degree macromonomer methyl allyl polyoxyethylene polyoxypropylene ether
  • Preparation method of block-type high polymerization degree macromonomer methyl allyl polyoxyethylene polyoxypropylene ether
  • Preparation method of block-type high polymerization degree macromonomer methyl allyl polyoxyethylene polyoxypropylene ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Preparation of 2-methyl-2-propenyl-1-ol polyoxyethylene (87.5) polyoxypropylene (10) ether

[0034] (1) Add 3780g of 2-methyl-2-propenyl-1-ol (52.5mol) and 50g of beaded sodium hydroxide into the external circulation ethoxylation reactor, dehydrate in vacuum for 1 hour, and replace with nitrogen three times, Turn on the circulation pump, gradually increase the temperature of the kettle to 100°C, and feed 46,200g of ethylene oxide. After the feed is complete, heat preservation and aging reaction for 0.5 hours, and then cool down to 60°C to obtain methyl alkenyl alcohol polyoxyethylene ether oligomerization substance (referred to as TPEG-20B).

[0035] (2) Add 10,000 g of the oligomer (TPEG-20B) obtained in step (1) and 52.3 g of sodium methoxide into the reactor, replace it with nitrogen three times, turn on the circulation pump, gradually raise the temperature to 100 ° C, and vacuum dealcoholize for 1 hour; Pass into 6090g of propylene oxide then, continue to insulate ...

Embodiment 2

[0038] Preparation of 2-methyl-2-propenyl-1-ol polyoxyethylene (110) polyoxypropylene (20) ether

[0039] (1) Add 2590g of 2-methyl-2-propenyl-1-ol (35.97mol) and 25g of sodium hydride into the external circulation ethoxylation reactor, vacuum dehydrate for 1 hour, replace with nitrogen three times, and turn on the circulation pump , gradually raise the temperature of the kettle to 80°C, feed 47,483g of ethylene oxide, and then heat-preserve and ripen the reaction for 1 hour after passing through completely, then cool down to 60°C, and send the intermediate (TPEG-30B for short) to The intermediate storage tank is protected with nitrogen gas.

[0040] (2) Add 11620g of the oligomer (TPEG-30B) obtained in step (1) and 285.8g of sodium hydroxide into a 60L external circulation ethoxylation reactor, replace it with nitrogen three times, turn on the circulation pump, and gradually raise the temperature To 130°C, vacuum dehydration for 0.5 hours; then 9683g of propylene oxide was p...

Embodiment 3

[0043] Preparation of 3-methyl-3-butenyl-1-ol polyoxyethylene (60) polyoxypropylene (10) ether

[0044] (1) Add 3050g 3-methyl-3-butenyl-1-ol (3-methyl-3-buten-1-ol, 35.46mol) and 74.6g methanol to the external circulation ethoxylation reactor Sodium, dealcoholized in vacuum for 1 hour, replaced with nitrogen three times, turned on the circulation pump, gradually increased the temperature of the kettle to 40°C, dealcoholized in vacuum for 1 hour, controlled the vacuum degree at -0.065MPa, and then began to introduce 15602g of ethylene oxide , After the feed is complete, heat preservation and aging reaction for 0.5 hours, the temperature is lowered to 60 ° C, and the intermediate (abbreviated as TPEG-10A) is sent to an intermediate storage tank with nitrogen pressure and protected with nitrogen.

[0045] (2) Add 5839g of the oligomer (TPEG-10A) obtained in step (1) and 264.6g of sodium methoxide into a 60L external circulation ethoxylation reactor, replace it with nitrogen thre...

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

PropertyMeasurementUnit
Hydroxyl valueaaaaaaaaaa
Hydroxyl valueaaaaaaaaaa
Hydroxyl valueaaaaaaaaaa
Login to View More

Abstract

The invention discloses a preparation method of block-type high polymerization degree macromonomer methyl allyl polyoxyethylene polyoxypropylene ether. The preparation method comprises the following steps: (1) using methyl allyl alcohol as an initiator, adding ethylene oxide in the presence of a basic catalyst to the methyl allyl alcohol so as to carry out condensation reaction, after completing addition, carrying out heat preservation and curing so as to obtain a methyl allyl alcohol polyoxyethylene ether low polymer; (2) adding the basic catalyst to the low polymer obtained in the step (1), adding the ethylene oxide so as to carry out condensation reaction, after completing addition, carrying out heat preservation and curing; and (3) continuously adding the ethylene oxide to a reactor so as to carry out condensation reaction till no pressure exists in the reactor, and then adding acetic acid for neutralization, thus obtaining the block-type high polymerization degree macromonomer methyl allyl polyoxyethylene polyoxypropylene ether. The preparation method has the advantages that the synthesis is carried out in two steps, the maximum weight increasing ratio can reach up to 1:100, the product is high in polymerization degree and reaction activity, and the slump retaining property and the combination property of the synthesized polycarboxylate-type water reducing agent are excellent.

Description

technical field [0001] The present invention relates to the synthesis of polyethers in organic chemistry. Background technique [0002] In recent years, my country's national economy has grown rapidly, and the construction industry has continued to develop rapidly. The construction of major projects such as high-speed railways, highways, airports, bridges, tunnels, hydropower, seaports and wharves has a high impact on high-performance concrete (HPC), self-compacting concrete (SCC), high-fluidity concrete (HFC), etc. are increasingly in demand, and the quality requirements are getting higher and higher, and the workability requirements for concrete mixtures are also integrated and diversified, such as high fluidity, slump Small loss, no bleeding, no segregation, good pumpability. [0003] After years of development, the water reducer products have gone through the early lignosulfonate (LS), the naphthalene-based water reducer (naphthalene sulfonate formaldehyde condensate BNS)...

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
no application Login to View More
IPC IPC(8): C08G65/28
Inventor 尹慧卿李森徐芳
Owner XINGTAI LANTIAN FINE CHEM
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com