Method for co-production of dimethyl decynediol and methyl hexynol

A technology of dimethyl decyne diol and methyl hexynol, which is applied in the field of co-production of dimethyl decyne diol and methyl hexynol, can solve the problems of high temperature, long reaction time and large molecular structure steric hindrance. and other problems, to achieve the effect of improving production efficiency, low reaction temperature, and inhibiting side reactions

Pending Publication Date: 2021-12-21
四川众邦新材料股份有限公司
View PDF9 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is little public information about the industrial synthesis of these two chemical substances. From the molecular structures of these two chemical substances, it can be known that both dimethyldecynediol and methylhexynol can be passed through Reppe with 2-pentanone and acetylene. However, the molecular structure of the raw material ha

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) Put 1750g of ethyl butyl ether as solvent and 250g of potassium tert-butoxide (industrial grade, purity 98%) into the grinder in order to grind it into a slurry, transfer it to the reaction kettle, start stirring, and heat to 70℃~ Keep at 80°C for 1 hour, then lower the temperature to 15°C to 20°C for control. Feed acetylene gas, keep the acetylene pressure in the range of 0.1MPa-0.12MPa, and react for 1.5 hours.

[0039] (2) Add 360g of 2-pentanone (industrial grade, purity 99.5%) into the reactor from the overhead tank evenly and slowly, and control the addition within 80-100 minutes, while keeping the acetylene pressure in the range of 01MPa-0.12MPa for reaction. After adding 2-pentanone, gradually raise the reaction temperature to 33°C to 35°C at a rate of 1°C to 2°C every about 10 minutes and keep it there. After the reaction lasted for about 3.5 hours, the residual 5-methyl-2-hexanone in the reaction material was sampled and detected to be less than 8%, and t...

Embodiment 2

[0048] The operation was carried out according to the operation method of Example 1, wherein: the feeding material in the operation step (1) was 2000 g of solvent n-butyl ether, and the catalyst was 140 g of potassium hydroxide (industrial grade, purity 94%). The pressure of acetylene is 0.1MPa~0.12MPa.

[0049] The feeding material in operation step (2) is 370 g of 2-pentanone (industrial grade, purity 99.5%), which is equivalent to 2-pentanone: potassium hydroxide (pure) = 1.1:1 (molar ratio). The pressure of acetylene is 0.12MPa~0.14MPa.

[0050] In the operation step (3), the feeding material is 2-pentanone (industrial grade, purity 99.5%) 268g, the total amount of 2-pentanone added twice: potassium hydroxide (pure) = 1.9:1 (molar ratio) . Control the entry temperature of the water medium at 78°C to 80°C; control the residence time of the reaction materials in the reaction tube for 1 to 1.5 minutes. The total amount of clear water used to terminate the reaction is about...

Embodiment 3

[0053] The operation was carried out according to the operation method of Example 1, wherein: the feed in the operation step (1) was 1800 g of solvent xylene, and the catalyst was 260 g of potassium isobutoxide (self-made, purity 97.5%). The pressure of acetylene is 0.1MPa~0.12MPa.

[0054] The feeding material in operation step (2) is 390 g of 2-pentanone (industrial grade, purity 99.5%), which is equivalent to 2-pentanone:potassium isobutoxide (purity)=1.21:1 (molar ratio). The pressure of acetylene is 0.08MPa~0.1MPa.

[0055] In the operation step (3), the feeding material is 2-pentanone (industrial grade, purity 99.5%) 208g, the total amount of 2-pentanone added twice: potassium isobutoxide (pure) = 1.85:1 (molar ratio ). Control the entry temperature of the water medium at 62°C to 64°C; control the residence time of the reaction materials in the reaction tube for 2.5 to 3 minutes. The total amount of clear water used to terminate the reaction is about 550g.

[0056] F...

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 relates to a method for co-production of dimethyl decynediol (4, 7-dimethyl-5-decyne-4, 7-diol) and methyl hexynol (3-methyl-1-hexyne-3-alcohol), which comprises the following steps: by taking 2-pentanone and acetylene as raw materials, potassium hydroxide or potassium isobutoxide or potassium tert-butoxide as a catalyst and an organic solvent as a dispersing agent, reacting 2-pentanone with normal-pressure or low-pressure acetylene at a relatively low temperature to generate a methyl hexynol-catalyst complex, mixing the methyl hexynol-catalyst complex with 2-pentanone, and quickly reacting through a high-temperature reaction tube to generate the dimethyl decynediol-catalyst complex; hydrolyzing the reaction product to remove potassium hydroxide, and fractionating to collect each part. The method has the characteristics of low reaction temperature, short reaction time, less side reaction, less catalyst consumption and the like.

Description

technical field [0001] The invention relates to a synthesis method of chemical substances 4,7-dimethyl-5-decyn-4,7-diol and 3-methyl-1-hexyn-3-ol. Background technique [0002] Both dimethyldecynediol (4,7-dimethyl-5-decyn-4,7-diol) and methylhexynol (3-methyl-1-hexyn-3-ol) It is a chemical intermediate with excellent surface activity. It is used alone or as one of the components. It is also an upstream raw material for the further synthesis of nonionic surfactants with unique properties. At present, there is little public information about the industrial synthesis of these two chemical substances. From the molecular structures of these two chemical substances, it can be known that both dimethyldecynediol and methylhexynol can be passed through Reppe with 2-pentanone and acetylene. However, the molecular structure of the raw material has a large steric hindrance, and the reaction process requires a higher temperature and a longer reaction time, which will inevitably lead to...

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): C07C33/044C07C33/042C07C29/42C07C29/74C07C29/88C07C29/80
CPCC07C29/42C07C29/74C07C29/88C07C29/80C07C33/044C07C33/042
Inventor 王南王林生李果张鸿曾健孔林李代军
Owner 四川众邦新材料股份有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap