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Method for preparing 1,4-cyclohexanedimethanol

A technology of cyclohexanedimethanol and dimethyl cyclohexanedicarboxylate, which is applied in the field of preparation of 1,4-cyclohexanedimethanol, which can solve the problem of wide grain size distribution range, poor catalytic activity stability, and catalyst crystallinity. Low-level problems, to achieve the effect of easy preparation, high catalytic activity, uniform and adjustable grain size distribution

Active Publication Date: 2012-03-21
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Generally speaking, the catalyst used in the production of 1,4-cyclohexanedimethanol is prepared by the traditional co-precipitation method, which mainly has technical defects such as low catalyst crystallinity, wide grain size distribution range, and poor stability of catalytic activity. If it is used for a long time It is necessarily expensive for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Accurately weigh Cu(NO 3 ) 2 ·6H 2 O, Zn(NO 3 ) 2 ·6H 2 O and Al(NO 3 ) 3 9H 2 O, prepare mixed salt solution with deionized water, Cu in the solution 2+ The molar concentration is 0.6mol / L, Zn 2+ The molar concentration of Al is 0.6mol / L, Al 3+ The molar concentration is 0.3mol / L. Dissolve sodium hydroxide and sodium sulfate in deionized water to prepare a mixed alkaline solution, wherein the molar concentration of sodium hydroxide is 2.4 mol / L, and the molar concentration of sodium salt is 0.6 mol / L. Pour an equal volume of 100mL mixed salt solution and mixed alkaline solution into the colloid mill at the same time, stir at a speed of 3000 rpm for 2 minutes, then centrifuge and wash with deionized water for 5 times until the pH reaches about 7, and then mix with 250mL water Add them together to a 500mL three-neck flask for crystallization at 60°C for 6 hours, and then naturally cool to room temperature. After filtration, washing, and drying at 60°C for 12 ...

Embodiment 2

[0026] Accurately weigh Cu(NO 3 ) 2 ·6H 2 O, Zn(NO 3 ) 2 ·6H 2 O and Al(NO 3 ) 3 9H 2 O, prepare mixed salt solution with deionized water, Cu in the solution 2+ The molar concentration of Zn is 0.8mol / L, Zn 2+ The molar concentration of Al is 0.8mol / L, Al 3+ The molar concentration is 0.8mol / L. Sodium hydroxide and sodium chloride were dissolved in deionized water to prepare a mixed alkaline solution, wherein the molar concentration of sodium hydroxide was 3.84 mol / L, and the molar concentration of sodium chloride was 1.6 mol / L. Pour an equal volume of 100mL mixed salt solution and mixed alkaline solution into a rotating liquid film reactor for nucleation reaction, stir at 5000 rpm for 5 minutes, then centrifuge and wash with deionized water 5 times until the pH reaches 7 Then add it together with 250mL of water into a 500mL three-neck flask for crystallization at 80°C for 24 hours, and then naturally cool to room temperature. After filtering, washing, and drying a...

Embodiment 3

[0029] Accurately weigh Cu(NO 3 ) 2 ·6H 2 O, Zn(NO 3 ) 2 ·6H 2 O and Al(NO 3 ) 3 9H 2 O, prepare mixed salt solution with deionized water, Cu in the solution 2+ The molar concentration of Zn is 1.2mol / L, Zn 2+ The molar concentration is 1.2mol / L, Al 3+ The molar concentration is 1.6mol / L. Sodium hydroxide and sodium chloride were dissolved in deionized water to prepare a mixed alkaline solution, wherein the molar concentration of sodium hydroxide was 6.4 mol / L, and the molar concentration of sodium chloride was 3.2 mol / L. Pour an equal volume of 100mL mixed salt solution and mixed alkaline solution into a homogenizer at the same time, stir at a speed of 6000 rpm for 10 minutes, then centrifuge and wash with deionized water for 5 times until the pH reaches about 7, and then mix with 250mL Water was added together into a 500mL three-neck flask for crystallization at 80°C for 24 hours, and then naturally cooled to room temperature. After filtration, washing, and dryin...

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Abstract

The invention relates to a method for preparing 1,4-cyclohexanedimethanol. The temperature of a catalyst bed layer is controlled to be from 150 to 150 DEG C, the operation pressure is controlled to be from 5.0MPa to 8.0MPa, 1,4-cyclohexanedicarboxylate dissolved in methyl alcohol is contacted with hydrogen with the existence of a polybasic composite metal oxide catalyst containing copper oxide, the proportion by weight of the methyl alcohol to the 1,4-cyclohexanedicarboxylate is equal to (0.1-9) to 1, the LHSV (Liquid Hourly Space Velocity) is 1-10h-1; H2 / DMCD (mol / mol) is 200-600, the flow of H2 is 17.7 to 177.4L / h, and the filling quantity of the catalyst is 3ml. The catalyst adopted in the method has the excellent properties of high dispersion, uniform crystallite dimension distribution, low cost, environment friendliness, and the like; the method is characterized in that the hydrogenation reaction pressure is low, the catalysis activity is high, and the like; and the selectivity of the 1,4-cyclohexanedimethanolcan be 95% to 98%.

Description

technical field [0001] The invention relates to a method for preparing 1,4-cyclohexanedimethanol by hydrogenating dimethyl 1,4-cyclohexanedicarboxylate. Background technique [0002] 1,4-Cyclohexanedimethanol (CHDM) is an important new raw material for polyester production in industry. The biggest application is to use 1,4-cyclohexanedimethanol as raw material to synthesize PETG copolyester, and then process it to obtain bottles, sheets and thick materials through extrusion or injection molding. The products have good transparency and impact resistance performance, abrasion resistance and corrosion resistance. Other unsaturated polyester resins modified and synthesized, with extremely low water absorption and good boiling water resistance, can be used to make high-quality coatings, lamination and injection resins; also have high electrical resistance and good corrosion resistance , Widely used in the production of resins for electronic products and insulated wires. [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/27C07C29/149B01J23/80
Inventor 史君李峰程光剑张敏黄集钺琼伟格石鸣彦娄阳贺俊海李志宇
Owner PETROCHINA CO LTD
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