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Process for preparing halohydrins

A technology of halogenated alcohols and hydrogen halides, which is applied in the field of preparation of halogenated alcohols, can solve the problems of uneven treatment of deactivators, high solid content of the treatment system, and inability to realize directional and efficient titanium supplementation, and achieve mild reaction conditions and high raw material The effect of high conversion rate and prolonging service life

Active Publication Date: 2022-03-11
CHINA PETROLEUM & CHEM CORP +1
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  • Claims
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AI Technical Summary

Problems solved by technology

Patent CN 102309983 A discloses a method for regenerating deactivated titanium-silicon molecular sieves. The deactivated titanium-silicon molecular sieves and regenerated rubber containing silicon, titanium, organic bases and water are treated at high temperature in a closed reactor for more than 2 hours to make the catalyst The activity is restored to the level of the fresh agent. This method must have silicon and titanium species at the same time, and it cannot achieve directional and efficient titanium supplementation. In addition, the solid content of the treatment system of this method is too high, which may cause uneven treatment of the deactivator
The regeneration methods of the existing catalysts are all aimed at the regeneration of the deactivator under neutral or alkaline conditions, and the regeneration of the deactivated catalyst for the preparation of the halohydrin catalyst under the acidic system, or the method of prolonging its service life has not been reported.

Method used

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  • Process for preparing halohydrins
  • Process for preparing halohydrins
  • Process for preparing halohydrins

Examples

Experimental program
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preparation example Construction

[0049] The preparation method of TS-1 molecular sieve is: the tetrapropyl ammonium hydroxide (TPAOH, 20%, purchased from U.S. Aldrich Company) solution of about 3 / 4 amount is added in tetraethyl orthosilicate (TEOS) solution, Obtain a liquid mixture with a pH of about 13, and then add a required amount of n-butyl titanate [Ti(OBu) dropwise to the obtained liquid mixture under vigorous stirring. 4 ] in anhydrous isopropanol solution, and after stirring for 15 minutes, a clear liquid was obtained. Finally, the remaining TPAOH was slowly added to the clear liquid, and stirred at 348-353K for about 3 hours to obtain a chemical composition of 0.03TiO 2 : SiO 2 :0.36TPA:35H 2 The sol of O was then crystallized at 443K for 3 days, and then the obtained solid was filtered, washed with distilled water, dried at 373K for 5 hours, and then calcined at 823K for 10 hours to obtain a molecular sieve sample. Wherein, the consumption of TEOS is 42g, the consumption of TPAOH is 73g, Ti(OBu) ...

Embodiment 1

[0055] The TS-1 molecular sieve catalyst is packed in a fixed bed reactor to form a TS-1 molecular sieve catalyst bed. Hydrogen peroxide, polymaleic anhydride (weight average molecular weight 5000) and water were mixed to form a liquid mixture. Then the liquid mixture, allyl chloride, and hydrochloric acid (37% aqueous solution) are passed into a fixed-bed reactor at the same time to contact and react with the TS-1 molecular sieve catalyst bed. Among them, among the reaction raw materials, allyl chloride: H 2 o 2 : Water (molar ratio) is 1:1.3:40, H 2 o 2 : HCl (molar ratio) is 1:1.5, chloropropene: polymaleic anhydride (weight ratio) is 1:0.008. The material weight hourly space velocity in the fixed bed reactor is 80h -1 , the catalyst bed temperature was 40°C, and the reaction was carried out continuously. During the reaction, the composition of the product at the outlet of the reactor was monitored by gas chromatography. The analysis results are shown in Table 1.

Embodiment 2

[0057] The TS-1 molecular sieve catalyst is packed in a fixed bed reactor to form a TS-1 molecular sieve catalyst bed. Hydrogen peroxide, polymaleic anhydride (weight average molecular weight 5000), tetrabutyl titanate and water were mixed to form a liquid mixture. Then the liquid mixture, allyl chloride, and hydrochloric acid (37% aqueous solution) are passed into a fixed-bed reactor at the same time to contact and react with the TS-1 molecular sieve catalyst bed. Among them, among the reaction raw materials, allyl chloride: H 2 o 2 : Water (molar ratio) is 1:1.3:40, H 2 o 2 : HCl (molar ratio) is 1:1.5, propylene chloride: polymaleic anhydride (weight ratio) is 1:0.008, polymaleic anhydride: tetrabutyl titanate (weight ratio) is 1:0.02. The material weight hourly space velocity in the fixed bed reactor is 80h -1 , the catalyst bed temperature was 40°C, and the reaction was carried out continuously. During the reaction, the composition of the product at the outlet of the...

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Abstract

The present disclosure relates to a method for preparing haloalcohols, the method comprising: contacting olefins, hydrogen halides, oxidants and protecting agents in the presence of a catalyst, wherein the catalyst is a titanium-silicon molecular sieve catalyst; the protecting agent It is a compound containing carbonyl and / or cyano, or, the protecting agent is a compound that can generate carbonyl and / or cyano during the reaction. The method has the advantages of simple operation process, mild reaction conditions, high raw material conversion rate and halogenated alcohol selectivity, and long service life of the catalyst.

Description

technical field [0001] The present disclosure relates to a method of preparing halohydrins. Background technique [0002] β-halohydrin has a substituted halogen atom on the carbon atom adjacent to the hydroxyl carbon, and is an important organic chemical intermediate. It can prepare epoxy compounds by saponification with alkali, and can be further used to prepare epoxy resins , polyols, polyether polyols and other important chemical products have broad market prospects. [0003] Common β-chlorohydrins include 2-chloroethanol, 1-chloro-2-propanol, 2-chloro-1-propanol, 3-chloro-1,2-propanediol, 2-chloro-1,3-propanediol , 1,3-dichloro-2-propanol, 2,3-dichloro-1-propanol, 2-chloro-1-cyclopentanol, 2-chloro-1-cyclohexanol, 2-chloro-1 -Cyclooctanol etc., they all can obtain corresponding epoxy compound by saponification reaction. [0004] The preparation methods of β-chlorohydrins in the prior art mainly include the chlorohydrination of olefins, the chlorination of allyl alcoho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/00C07C29/03C07C29/48C07C29/62C07C31/36B01J29/89
Inventor 彭欣欣夏长久朱斌林民罗一斌慕旭宏舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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