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Solid carbon sulfonic acid catalyst, preparation method thereof, tributyl citrate, and preparation method of tributyl citrate

A technology of tributyl citrate and carbon sulfonic acid is applied in the field of plasticizers to achieve the effects of improving stability and improving repeatability

Active Publication Date: 2020-03-13
HUAIHUA UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Based on this, it is necessary to provide a solid carbon sulfonic acid catalyst and a preparation method thereof, tributyl citrate and a preparation method thereof for the problem of how to improve the repeated practicability of the catalyst

Method used

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  • Solid carbon sulfonic acid catalyst, preparation method thereof, tributyl citrate, and preparation method of tributyl citrate
  • Solid carbon sulfonic acid catalyst, preparation method thereof, tributyl citrate, and preparation method of tributyl citrate
  • Solid carbon sulfonic acid catalyst, preparation method thereof, tributyl citrate, and preparation method of tributyl citrate

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preparation example Construction

[0037] The preparation method of the solid charcoal sulfonic acid catalyst of one embodiment, comprises the steps:

[0038] S10, soaking the bamboo powder in sodium silicate solution for 15h-20h, then soaking the bamboo powder in deionized water to achieve adsorption equilibrium, filtering and drying, and then heat-treating at 130°C-150°C for 3h-5h, Bamboo powder after alkaline pretreatment is obtained.

[0039] Preferably, bamboo powder is prepared through the following steps:

[0040] Bamboo is used as raw material, after being washed with water and dried, it is successively ground in a pulverizer, sieved with a sieve of 50 mesh to 70 mesh, and vacuum dried at a temperature of 50 DEG C to obtain bamboo powder.

[0041] The purpose of alkaline pretreatment of bamboo powder is to make sodium silicate saturated and adsorbed in the structure of bamboo powder, so that there will be no residual sodium silicate attached to the surface of bamboo powder.

[0042] S20. Mix the alkal...

Embodiment 1

[0066] The preparation of embodiment 1 solid charcoal sulfonic acid catalyst

[0067] The bamboo powder pulverized with pulverizer is sieved with 60 mesh sieves, and vacuum-dried at 50 ℃ of temperature. After cooling, the bamboo powder is taken out, and the dry bamboo powder of 10g is weighed rapidly. Bamboo powder was soaked in 10% sodium silicate solution by equal-volume immersion method, soaked for 16 hours, then soaked in deionized water to reach adsorption equilibrium, filtered and dried, and passed water vapor in tube furnace for 140 ℃ heat treatment for 4h.

[0068] Add hydrochloric acid to the bamboo powder after alkaline pretreatment with sodium silicate to adjust the pH, so that the sodium silicate in the bamboo powder is converted into silicic acid. The bamboo powder was treated with 5% p-toluenesulfonic acid, heat treated with water vapor at 140° C. in a tube furnace, and then heated to 200° C. for 2 hours to obtain a pretreated composite bamboo material.

[006...

Embodiment 2

[0071] The preparation of embodiment 2 tributyl citrate

[0072] Add 0.1mol citric acid and 0.45mol n-butanol in a molar ratio to a 150ml three-necked flask equipped with a water separator, a thermometer, a reflux condenser and a stirring bar, then add 0.1g of solid carbon sulfonic acid catalyst, mix well, and simultaneously take Record the acid value of the reaction solution before the reaction, heat and stir with a collector-type constant temperature heating magnetic stirrer, stir to raise the temperature to a certain value, keep this temperature and reflux for 4 hours, and regularly take samples to measure the acid value of the reaction solution (according to GB / T1668 [93] method).

[0073] Heat the three-necked bottle with a water separator and a reflux device until the reflux starts to calculate the time, and stop the reaction when no water drops are separated. After the product is cooled and dipped, pour out the reaction solution and first recover n-butanol by normal pr...

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Abstract

The invention relates to a solid carbon sulfonic acid catalyst, a preparation method thereof, tributyl citrate, and a preparation method of tributyl citrate. The preparation method of the solid carbonsulfonic acid catalyst comprises the following steps: soaking bamboo powder in a sodium silicate solution for 15-20 h, then soaking the bamboo powder in deionized water to reach adsorption equilibrium, then filtering and drying the soaked bamboo powder, and then carrying out heat treatment at 130-150 DEG C for 3-5 h to obtain alkaline-pretreated bamboo powder; mixing the alkaline-pretreated bamboo powder with hydrochloric acid, adding p-toluenesulfonic acid after a reaction is completed, performing mixing until uniformity, and carrying out heat treatment at 140-200 DEG C for 1-3 h to obtain acidic-pretreated bamboo powder; and the acidic-pretreated bamboo powder is carbonized to obtain carbonized bamboo powder; and the carbonized bamboo powder is sulfonated to obtain the solid carbon sulfonic acid catalyst.

Description

technical field [0001] The invention relates to the technical field of plasticizers, in particular to a solid carbon sulfonic acid catalyst and a preparation method thereof, tributyl citrate and a preparation method thereof. Background technique [0002] Since the structure of the widely used plasticizer phthalate diester contains a carcinogenic risk of benzene ring, the country has formulated corresponding regulations to limit its use in food packaging materials, and recommend the use of non-toxic green citric acid three butyl ester (TBC). TBC is obtained by esterification of citric acid and n-butanol under the action of an acid catalyst. In the past ten years, many scholars have studied the heterogeneous acid catalysis process of new acid catalysts, and solid acid catalysts are one of them. The solid acid catalyst hopes to change the original homogeneous acid catalysis process into a heterogeneous acid catalysis process, thereby simplifying the separation of the catalyst...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J35/10B01J37/00B01J37/08C07C67/08C07C69/704
CPCB01J37/0009B01J37/084B01J31/0225C07C67/08B01J2231/49B01J35/613B01J35/633B01J35/647C07C69/704
Inventor 曾瞬钦罗琼林郑鑫鑫欧阳跃军舒友
Owner HUAIHUA UNIV
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