Method of preparing hydronol

A technology of isosorbide and sorbitol, which is applied in the field of isosorbide preparation from biomass raw materials, can solve the problems of reduced reaction rate, narrow operating temperature range, and difficult removal of ions, and achieves simple reaction operation process, obvious catalytic effect, and easy Effects of Separation and Recycling

Inactive Publication Date: 2009-07-29
青州市瑞鑫再生资源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are some common deficiencies in these production processes: kettle reaction, which requires dehydration under certain pressure or vacuum conditions, is not suitable for continuous production; inorganic acid as a catalyst has higher requirements for catalytic reactors, long life but easy to generate dark by-products Product, although the ion exchange resin produces few by-products, its service life is short; the operating temperature range is narrow, high temperature can easily lead to sorbitol decomposition or product carbon deposition, and low temperature can easily cause the water generated by t

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0017] Example 1

[0018] 64.4g ZrOCl 2 ·8H 2 O was dissolved in 500 ml of water, 28% ammonia water was added dropwise until the pH of the solution was 8.4, suction filtered and washed with deionized water until no Cl - exists, the resulting Zr(OH) 4 The filter cake was transferred to an oven at 120°C for drying for 24h, and then calcined at 500°C for 5h to obtain ZrO 2 .

[0019] Take 7.3972g ZrO 2 Add 6.7mL of 1M H 3 PO 4 , add a little water, heat and stir in a water bath at 80°C until it evaporates to dryness, dry at 100°C, then heat to 600°C within 3 hours, and calcine at 600°C for 4 hours to obtain PO with a molar ratio of P / Zr=1:9 4 3- / ZrO 2 catalyst. Cool down and cool, press into pieces and smash into 30-50 mesh sieves.

[0020] The above-mentioned 30-50 mesh P / Zr=1:9 PO 4 3- / ZrO 2 2.0 g of catalyst was charged into the constant temperature section of the tubular fixed bed reactor, and the rest was filled with quartz sand. After the system checks the ...

Example Embodiment

[0021]Example 2

[0022] Take the ZrO prepared according to the method of Example 1 2 7.3972g add 15.0mL 1M H 3 PO 4 , add a little water, heat and stir in a water bath at 80 °C until it evaporates to dryness, dry at 120 °C, then heat to 600 °C within 3 hours, and calcine at 600 °C for 6 hours to obtain PO with P / Zr=2:8 4 3- / ZrO 2 catalyst. Cool down and cool, press into pieces and smash into 30-50 mesh sieves.

[0023] The above-mentioned 30-50 mesh P / Zr=2:8 PO 4 3- / ZrO 2 2.0 g of catalyst was charged into the constant temperature section of the tubular fixed bed reactor, and the rest was filled with quartz sand. After the system checks the seal, the volume air velocity is 6h -1 N 2 The temperature of the catalytic bed was programmed to 250 °C under the gas flow rate, and then 10% sorbitol solution was injected into the system, and the reaction was carried out through the catalytic bed after gasification. The liquid samples collected after the reaction for 2 h w...

Example Embodiment

[0024] Example 3

[0025] Take 7.3972g ZrO prepared according to the method of Example 1 2 Add 25.7mL of 1M H 3 PO 4 , add a little water, heat and stir in a water bath at 80 °C until it evaporates to dryness, dry at 100 °C, then heat to 650 °C within 3 hours, and calcine at 650 °C for 4 hours to obtain PO with P / Zr=3:7 4 3- / ZrO 2 catalyst. Cool down and cool, press into pieces and smash into 30-50 mesh sieves.

[0026] The above-mentioned 30-50 mesh P / Zr=3:7 PO 4 3- / ZrO 2 2.0 g of catalyst was charged into the constant temperature section of the tubular fixed bed reactor, and the rest was filled with quartz sand. After the system checks the seal, the volume air velocity is 1h -1 N 2 The temperature of the catalytic bed was programmed to 350 ° C under the gas flow rate, and then 15% sorbitol solution was injected into the system, and the reaction was carried out through the catalytic bed after gasification. The liquid samples collected after the reaction for 2 h ...

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PUM

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Abstract

The invention discloses a preparation method of isobide. Sorbierite is used as raw material and H3PO4 modified tetravalent metal oxides are used as catalyst to prepare the isobide by the dehydration reaction. The method has the advantages of simple operation process, low production cost, little environmental pollution, easy separation and recovery. The used modified catalyst has obvious catalytic effect. The selectivity of the isobide reaches as high as 63.49 percent, and the yield reaches as high as 62.23 percent. With strong practicality, the method is novel and can satisfy the industrialization requirements.

Description

technical field [0001] The invention relates to the field of chemical technology, in particular to a 3 PO 4 The modified tetravalent metal oxide is used as a catalyst, and the method for preparing isosorbide by adopting biomass raw materials. Background technique [0002] Isosorbide is a dehydrated derivative of D-sorbitol. In medicine, sorbitol is an excellent antihypertensive drug and diuretic for the treatment of intracranial hypertrophy. After dehydration, the hydroxyl group becomes an ether bond, and its fat solubility is greatly increased. Already completely different from sorbitol, absorbed immediately after oral administration is an effective osmotic oral dehydration diuretic. Isosorbide has been used clinically in foreign countries, but in China it is only used as an intermediate for the synthesis of anti-anginal drugs isosorbide dinitrate and isosorbide mononitrate. Isosorbide is an important raw material and intermediate of span and Tween surfactants in industr...

Claims

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Application Information

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IPC IPC(8): C07D493/04B01J21/06B01J23/14B01J27/16A61P9/12A61P7/10
Inventor 黄和余定华顾铭燕
Owner 青州市瑞鑫再生资源科技有限公司
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