Acid-adjusting hydrolysis process for preparing levulinic acid
A technology for adjusting levulinic acid and acid, which is applied in the preparation of carboxylate salts, chemical instruments and methods, and the preparation of organic compounds. Effects of increasing production cost and technical difficulty, shortening hydrolysis time, and increasing cellulose content
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[0019] Example 1:
[0020] 1. Raw materials: cellulose 40.13% corn stover; sulfuric acid 98%, analytically pure.
[0021] 2. Preparation:
[0022] (1) Raw material pretreatment: air-dried, crushed corn stalks, and passed through a 30-mesh sieve. (3) Hydrolysis: use dilute sulfuric acid as a catalyst, add 2000ml of dilute sulfuric acid solution with a mass concentration of 3.8%, add corn stalks at a solid-liquid ratio of 1:19.5, stir evenly, and let stand at room temperature for 30 minutes to mix the material and liquid. It was heated to 239.5°C within 3.2 minutes, and reacted for 34.3 minutes under the conditions of 239.5°C and 2.4 mPa pressure at a rotation speed of 100 r / min. (4) Acid adjustment: quickly cool down to 50°C, reduce to normal pressure, reduce the speed to 70r / min, inject 20ml of 20% sulfuric acid solution, and then quickly raise the temperature to 205°C, speed 160r / min, reaction pressure 2.2mPa, reaction time 20 minutes. (5) Target product detection: the reaction ...
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[0023] Example 2:
[0024] 1. Raw material: 36.2% cellulose rice straw; 98% sulfuric acid, analytically pure.
[0025] 2. Preparation:
[0026] (1) Raw material pretreatment: air-dry and crush the rice straw, and pass through a 30-mesh sieve; (3) Hydrolysis: use dilute sulfuric acid as a catalyst, add 2000ml of dilute sulfuric acid solution with a mass concentration of 3.9%, and add the rice at a solid-liquid ratio of 1:17.4 Stir and stir evenly, and let stand at room temperature for 30 minutes to make the material and liquid fully mixed. It is heated to 241.2°C within 3.5 minutes, and reacted for 34.5 minutes under the conditions of 241.2°C and 2.4 mPa pressure at a rotation speed of 120r / min. (4) Acid adjustment: quickly cool down to 50°C, reduce to normal pressure, speed down to 70r / min, inject 20ml of 20% sulfuric acid solution, and then quickly heat up to 205°C, speed 160r / min, reaction pressure 2.2mPa, reaction time 20 minutes. (5) Target product detection: the reaction is ...
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[0027] Example 3:
[0028] 1. Raw materials: combined raw materials: corn stover 40%, rice straw 40%, rice husk 20%, the average cellulose content after mixing is 35.15%; sulfuric acid 98%, analytically pure.
[0029] 2. Preparation:
[0030] (1) Raw material pretreatment: Corn straw, rice straw, and rice husk are air-dried, crushed, passed through a 30-mesh sieve, and the three raw materials are combined at 2:2:1. (3) Hydrolysis: using dilute sulfuric acid as a catalyst, adding 2000ml of dilute sulfuric acid solution with a mass concentration of 3.7%, adding the combined raw materials according to the solid-liquid ratio of 1:17.9, stirring uniformly, and letting it stand at room temperature for 30 minutes to fully mix the material and liquid. It was heated to 233.1°C in 3.8 minutes, and reacted for 32.1 minutes under the conditions of 233.1°C and 2.3 mPa pressure at a speed of 110 r / min. (4) Acid adjustment: quickly cool down to 50°C, reduce to normal pressure, speed down to 70r / m...
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