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Method for one-step hydration synthesis of terpilenol by catalyzing turpentine through carbon-based solid acid

A technology of carbon-based solid acid and turpentine, which is applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve problems such as catalyst activity and preparation process difficulties, complicated preparation of supported catalysts, difficulty in homogeneous catalytic recovery, etc. , to achieve the effects of easy regeneration, high yield and selectivity, and reduced production costs

Active Publication Date: 2015-04-22
GUANGXI UNIV FOR NATITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Inorganic acids and organic acids have the disadvantages of many side reactions, low yield, difficult recovery, and a large amount of post-treatment wastewater; organic acids and heteropoly acids have problems such as difficult recovery of homogeneous catalysis, complicated preparation of supported catalysts, and high cost; fresh Cation exchange resins show good catalytic activity, but after repeated reuse, the catalytic efficiency decreases, regeneration is difficult, and the waste catalyst produced causes environmental pollution; on the one hand, ionic liquids and solid superacids are expensive, and at the same time, the preparation of catalysts is complicated, and the catalyst activity It is difficult to control the preparation process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The method utilizing carbon-based solid acid to synthesize terpineol:

[0024] (1) Preparation of carbon-based solid acid catalyst: Take 100 parts by weight of wood pulp alkali lignin, 2 parts of sodium hydroxide, and 100 parts of water into the reaction kettle, stir and dissolve at room temperature, and then add 10 parts of epoxy chloride Propane, stirred for 1 hour, gelatinized at 30°C for 24 hours, soaked in hydrochloric acid aqueous solution with a concentration of 1mol / L for 10 hours, washed with water until neutral, dried in vacuum at 50°C for 24 hours, carbonized the dry gel at 300°C for 10 hours, Then use 98% concentrated sulfuric acid for sulfonation at 100°C for 10 hours. During sulfonation, 100 parts by weight of carbon are sulfonated with 180 parts by weight of 98% concentrated sulfuric acid. After sulfonation, wash with deionized water to neutrality. Vacuum-dried at 50°C for 24 hours to obtain a carbon-based solid acid catalyst.

[0025] (2) Hydration rea...

Embodiment 2

[0028] The method utilizing carbon-based solid acid to synthesize terpineol:

[0029] (1) Preparation of carbon-based solid acid catalyst: Take 100 parts by weight of bamboo pulp alkali lignin, 10 parts of sodium hydroxide, and 200 parts of water into the reaction kettle, stir and dissolve at room temperature, and then add 50 parts of epoxy chloride Propane, stirred for 1 hour, gelatinized at 40°C for 20 hours, soaked in hydrochloric acid solution with a concentration of 1mol / L for 14 hours, washed with water until neutral, dried in vacuum at 60°C for 20 hours, carbonized the dry gel at 350°C for 8 hours, Then use 98% concentrated sulfuric acid for sulfonation at 120°C for 8 hours. During sulfonation, 100 parts by weight of carbon is sulfonated with 200 parts by weight of 98% concentrated sulfuric acid. After sulfonation, it is washed with deionized water to neutrality. Vacuum-dried at 60°C for 20 hours to obtain a carbon-based solid acid catalyst.

[0030] (2) Hydration r...

Embodiment 3

[0033] The method utilizing carbon-based solid acid to synthesize terpineol:

[0034] (1) Preparation of carbon-based solid acid catalyst:

[0035] Take 100 parts by weight of straw pulp alkali lignin, 20 parts of sodium hydroxide, and 300 parts of water into the reaction kettle, stir and dissolve at room temperature, add 150 parts of epichlorohydrin, stir for 1 hour, and gel at 60°C 16h, soak the gel in 1mol / L hydrochloric acid aqueous solution for 18h, wash with water until neutral, dry in vacuum at 70°C for 18h, carbonize the dry gel at 400°C for 7h, then use 98% concentrated sulfuric acid at 140°C Sulfonate for 6 hours, sulfonate 100 parts by weight of carbon with 220 parts by weight of 98% concentrated sulfuric acid, wash with deionized water to neutrality after sulfonation, and dry in vacuum at 70°C for 18 hours to obtain carbon-based solid acid catalyst.

[0036] (2) Hydration reaction: Take 2 parts of carbon-based solid acid catalyst, 15 parts of distilled water,...

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Abstract

The invention provides a method for one-step hydration synthesis of terpilenol by catalyzing turpentine through carbon-based solid acid. The method is characterized in that the turpentine is used as the raw material, isopropyl alcohol or butyl alcohol or isobutyl alcohol is used as the solvent, and the terpilenol is formed by means of one-step hydration synthesis through the turpentine under the catalytic action of a carbon-based solid acid catalyst. The carbon-based solid acid is prepared through a lignin gel method and has the advantages of developed micropores and mesopores, high catalytic activity, easy separation, good thermostability, repeatable utilization, easy regeneration, low preparation cost and the like; since the carbon-based solid acid is used for catalyzing the turpentine to form the terpilenol by means of one-step hydration synthesis, the conversion rate of the turpentine is up to 95-98 percent, and the yield of the terpilenol is 35-42 percent; besides, in the production process, no liquid waste acid or waste water is produced, pollution to the environment is greatly relieved, and the requirement for green chemistry is met.

Description

technical field [0001] The invention relates to a method for synthesizing terpineol, in particular to a method for synthesizing terpineol by one-step hydration of turpentine catalyzed by a carbon-based solid acid. Background technique [0002] Terpineol has a lilac aroma and is widely used in the perfume industry, mainly used in soaps, cosmetic fragrances and blending essences; terpineol containing 40% to 85% alcohol is mainly used as foaming in the non-ferrous metal flotation industry In addition, terpineol can also be used in industries such as medicine, detergent, ink, instrumentation, and telecommunications. Terpineol is also an important chemical raw material. Natural terpineol exists in a small amount and cannot meet industrial needs, so it is mainly synthesized artificially. Synthetic terpineol is obtained from turpentine oil through acid-catalyzed hydration. Traditional terpineol synthesis process route mainly contains two: the first route is a one-step method, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/14C07C29/04B01J27/02
CPCB01J27/02C07C29/04C07C29/60C07C29/80C07C2601/16C07C33/14
Inventor 刘祖广曹松卢祥雷福厚
Owner GUANGXI UNIV FOR NATITIES
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