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New technology for preparing flaky borneol from synthetic borneol crystals

A technology for synthesizing borneol and a new process, which is applied in the separation/purification of hydroxyl compounds, organic chemistry, etc., can solve the problem of low yield of borneol, and achieve the effect of improving the yield

Active Publication Date: 2015-11-11
福建南平青松化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The invention provides a new process for preparing borneol flakes by synthesizing borneol crystals, which overcomes the shortcoming of the low yield of borneol flakes in the existing synthetic borneol crystallization process, and can effectively increase the yield of borneol flakes produced by synthesizing crude borneol crystals

Method used

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  • New technology for preparing flaky borneol from synthetic borneol crystals
  • New technology for preparing flaky borneol from synthetic borneol crystals
  • New technology for preparing flaky borneol from synthetic borneol crystals

Examples

Experimental program
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Effect test

Embodiment 1

[0027] The steps of the new technique for preparing borneol crystals from synthetic borneol crystals are as follows:

[0028] 1. Break the synthetic borneol block crude product into small pieces, weigh 800g and add it to the jacketed reaction flask, install a thermometer and a stirring rod, then add 1200g p-cymene, heat up to 90°C and slowly stir to dissolve;

[0029] 2. Stop stirring, gradually lower the temperature of the dissolved material to the first precipitation temperature of 60°C, and keep the temperature constant for 1 hour;

[0030] 3. After the heat preservation is over, cool down to the second precipitation temperature of 40°C at 0.5°C / h, and keep the material at the second precipitation temperature for 8 hours;

[0031] 4. After the heat preservation is over, cool down at 0.25°C / h, and drain the hot water in the jacket until it cools down to room temperature;

[0032] 5. After 7 days of natural cooling and crystallization, put the gasoline in the reaction bottle...

Embodiment 2

[0035] The steps of the new technique for preparing borneol crystals from synthetic borneol crystals are as follows:

[0036] 1. Break the synthetic borneol massive crude product into small pieces, weigh 800g and put it into the jacketed reaction bottle, install a thermometer and a stirring rod, then add 1300g of 120# gasoline, heat up to 120°C and slowly stir to dissolve;

[0037] 2. Stop stirring, gradually lower the temperature of the dissolved material to the first precipitation temperature of 90°C, and keep the temperature constant for 24 hours;

[0038] 3. After the heat preservation is over, cool down to the second precipitation temperature of 45°C at 0.25°C / h, and keep the material at the second precipitation temperature for 10 hours;

[0039] 4. After the heat preservation is over, cool down at 0.25°C / h, and drain the hot water in the jacket until it cools down to room temperature;

[0040] 5. After 7 days of natural cooling and crystallization, put the 120# gasoline...

Embodiment 3

[0043] The steps of the new technique for preparing borneol crystals from synthetic borneol crystals are as follows:

[0044] 1. Break the synthetic borneol block crude product into small pieces, weigh 800g and put it into a jacketed reaction flask, install a thermometer and a stirring rod, then add 960g of ethanol, heat up to 120°C and slowly stir to dissolve;

[0045] 2. Stop stirring, gradually lower the temperature of the dissolved material to the first precipitation temperature of 120°C, and keep the temperature constant for 48 hours;

[0046] 3. After the heat preservation is over, cool down to the second precipitation temperature of 75°C at 1°C / h, and keep the material at the second precipitation temperature for 6 hours;

[0047] 4. After the heat preservation is over, cool down at 1°C / h, and drain the hot water in the jacket until it cools down to room temperature;

[0048] 5. After 5 days of natural crystallization, put the ethanol in the reaction bottle into the rec...

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Abstract

The invention relates to a new technology for preparing flaky borneol from synthetic borneol crystals. The new technology comprises the following steps: 1) crushing materials; 2) dissolving the materials, namely mixing an organic solvent used for dissolving synthetic borneol with the synthetic borneol in a weight ratio of (0.9-20):1, and stirring while heating until the synthetic borneol is dissolved; 3) carrying out gradient temperature control precipitation, namely gradually cooling the dissolved materials to a first precipitation temperature of 50-120 DEG C, and then cooling to a second precipitation temperature of 40-80 DEG C at a rate of 0.05-2 DEG C / h; and 4) cooling and crystallizing, namely cooling to room temperature at a rate of 0.05-2 DEG C / h or freezing and cooling to the temperature ranging from -5 DEG C to -15 DEG C at a rate of 0.2-5 DEG C / h, crystallizing for a plurality of days, precipitating flaky synthetic borneol in the materials, and drying, so that a flaky synthetic borneol finished product is obtained. The new technology has the advantages that the defect that the yield of flaky borneol of an existing synthetic borneol crystallization technology is low is overcome, and the yield of the synthetic borneol crude product, namely flaky borneol, can be effectively improved.

Description

technical field [0001] The invention relates to a new process for preparing borneol flakes by synthesizing borneol crystals, which is applied to the purification of synthetic borneol crude products. Background technique [0002] Borneol, also known as borneol, is divided into natural borneol and synthetic borneol. Natural borneol is mainly derived from natural crystalline compounds precipitated from dipterocarp tree resin, which is a genuine product in borneol, but natural borneol resources are in short supply and can no longer meet social needs. Therefore, synthetic borneol is currently used to replace natural borneol. ice flakes. The most widely used method of synthesizing borneol in industry, its main principle is to use an acid (or acid anhydride) to react with α-pinene under certain conditions to generate ester (rearrangement-addition reaction), then saponification reaction occurs, and hydrolysis produces Orthoborneol and isoborneol are subjected to a series of post-t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C35/30C07C29/74C07C29/78
CPCC07C29/76C07C29/78C07C35/30
Inventor 江承艳熊开斌杨伟斌
Owner 福建南平青松化工有限公司