Preparation method of dimethyl adipate and lignin carbon-based solid acid catalyst

A technology of dimethyl adipate and solid acid catalyst, which is applied in the direction of carboxylic acid ester preparation, organic compound preparation, physical/chemical process catalyst, etc., and can solve the problem of long reaction time, high esterification temperature, There are many by-products of methyl esters, etc., to achieve the effect of reducing energy consumption and saving resources

Pending Publication Date: 2022-04-19
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Patent CN109748791B discloses an energy-saving method for producing dimethyl adipate, which uses methanol and molten adipic acid as raw materials, strong acidic cation exchange resin as catalyst, and adopts continuous stirring reactor and esterification reaction rectification The tower carries out primary and secondary esterification reactions. Although the conversion rate of this preparation method is high, there are many by-products in the preparation of dimethyl adipate by this method, and the esterification temperature is high and the reaction time is long.

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  • Preparation method of dimethyl adipate and lignin carbon-based solid acid catalyst
  • Preparation method of dimethyl adipate and lignin carbon-based solid acid catalyst
  • Preparation method of dimethyl adipate and lignin carbon-based solid acid catalyst

Examples

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Effect test

Embodiment 1

[0038] This embodiment introduces the amount of fixing adipic acid, methanol and reaction temperature, and by changing the amount of catalyst, the influence of the amount of catalyst on the conversion rate of adipic acid and the yield of dimethyl adipate is obtained:

[0039] Such as figure 1 As mentioned above, in this embodiment, the amount of adipic acid is selected as 0.1 mol, the ratio of methanol to adipic acid is 7:1, the reaction temperature is 73°C, and the amount of catalyst is 5% of the mass of adipic acid. 8%, 10%, 12%, 15%, 17%, 20%, and 22% were used for batch catalysis experiments.

[0040] With the increase of the amount of catalyst, the catalytic effect is also gradually improved. Among them, the amount of catalyst has little influence on the conversion rate of adipic acid, which reaches about 90% in 50 minutes; while the effect on the yield of DMA is more obvious. The yield increased from 63.93% to 98.15% in 120 minutes. As the amount of catalyst added reac...

Embodiment 2

[0043] This example describes the effect of fixing the amount of adipic acid and constant reaction temperature, and changing the amount of methanol to obtain the influence of different acid-alcohol molar ratios on the yield of DMA and the conversion rate of adipic acid:

[0044] Such as figure 2 As shown, in order to maximize the conversion of the raw material adipic acid and to suppress the reverse reaction, an excess of methanol is selected. The amount of adipic acid is selected as 0.1mol as a benchmark, and when the reaction temperature is 73°C and the catalyst dosage is 20% of the mass of adipic acid, the alkyd-acid molar ratio is 4:1, 5:1, 6:1 , 7:1, 8:1, and 9:1 were used for catalytic experiments.

[0045] Experimental results such as figure 2 , image 3 shown, where figure 2 a and b show the change of DMA yield and adipic acid conversion rate with time under different alkyd ratios. Since the range of change is too small, the data at 120 minutes were taken for gr...

Embodiment 3

[0047] This embodiment has introduced the consumption of fixing adipic acid, methyl alcohol, catalyst, by changing reaction temperature, measures the impact of reaction temperature on the conversion rate of adipic acid and the yield of DMA:

[0048] Such as Figure 4 As shown, in order to determine the optimal temperature, the amount of catalyst is 20% of the mass of adipic acid, the molar ratio of alkyd to acid is 8:1, and the selected temperatures are 58°C, 63°C, 68°C, and 73°C for catalytic experiments. According to the experimental results, the conversion rate of adipic acid and the yield of DMA at the end of the reaction were selected as benchmarks.

[0049] From the experimental results, it can be concluded that as the temperature increases, the conversion rate of adipic acid and the yield of DMA both increase. In theory, the higher the temperature is, the more favorable the reaction is. At normal pressure, at 73°C, the bubble point temperature of the reaction has been ...

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Abstract

The invention provides a preparation method of dimethyl adipate and a lignin carbon-based solid acid catalyst, reaction raw materials for preparing the dimethyl adipate comprise methanol, adipic acid and the lignin carbon-based solid acid catalyst, in an esterification reaction of the dimethyl adipate, the yield of the dimethyl adipate can reach 98%, the conversion rate of the adipic acid can reach 99%, and the yield of the lignin carbon-based solid acid catalyst can reach 98%. And compared with other solid acid catalysts, the lignin carbon-based solid acid catalyst has a more excellent effect of catalyzing the reaction, and can reach a higher esterification level within a shorter time and at a lower temperature, thereby greatly reducing the energy consumption and saving the resources.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and in particular relates to a preparation method of dimethyl adipate and a lignin carbon-based solid acid catalyst. Background technique [0002] Dimethyl adipate (DMA) is an important fine chemical product, which can be compatible with cellulose, chlorinated rubber, etc., so that it can be used to produce high-grade paint, synthetic resin, washing liquid and other chemical products. In addition, DMA can also be used as an intermediate in the synthesis of medicines, and can be used to synthesize 1,6-hexanediol through hydrogenation. The synthesis methods of DMA mainly include adipic acid and methanol synthesis method, cyclopentanone and dimethyl carbonate synthesis method, etc. Among them, the method of synthesizing DMA by the esterification reaction of adipic acid and dimethyl ester is commonly used in industry. The most commonly used catalysts for industrial esterification reacti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/75B01J27/02
CPCC07C67/08B01J27/02C07C2601/14C07C69/75
Inventor 方静张阳李浩
Owner HEBEI UNIV OF TECH
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