CN1114956A

CN1114956A - Extraction of natural guaiacol

Info

Publication number: CN1114956A
Application number: CN 93102022
Authority: CN
Inventors: 罗富源; 吴联真
Original assignee: Individual
Current assignee: Individual
Priority date: 1993-02-18
Filing date: 1993-02-18
Publication date: 1996-01-17
Anticipated expiration: 2013-02-18
Also published as: CN1040744C

Abstract

The natural guaiacol for production of high-quality vanillin is prepared from creosote as forest chemical product through such steps as salt-generating, filtrating, acidizing and rectifying. Its purity is above 95% and its extracting rate is over 60%.

Description

Extraction of natural guaiacol

The guaiacol is prepared by adopting a synthesis process at present in China, the purity of the obtained guaiacol is low, the cost is high, one raw material, namely the o-nitrochlorobenzene is imported, and the o-nitrochlorobenzene is converted into o-aminoanisole by a special factory after being imported to be used.

The natural guaiacol is widely present in hardwood dry distillation oil, the content of the pine root dry distillation impure phenol is up to 26 percent, the natural guaiacol is not developed and utilized all the time, and most of the natural guaiacol is burnt out along with light oil asfuel; some dry distillation turpentine oil manufacturers directly discharge the fusel oil into rivers due to no market for the miscellaneous phenols, thereby polluting the environment. The invention aims to extract natural guaiacol by completely adopting domestic raw and auxiliary materials, improve the purity and find an extraction process.

After repeated exploration for several years, four processes for extracting natural guaiacol have been researched;

the first is a calcium salt method, and the reaction formula is as follows:

filtering, washing, acid separating, washing and rectifying the calcium guaiacol precipitate to obtain the natural guaiacol product.

The second method is a magnesium salt method, and the reaction formula is as follows:

filtering, washing, acid separating, washing again and rectifying the guaiacol magnesium salt precipitate to obtain the natural guaiacol.

The two methods for extracting natural guaiacol are characterized by that it utilizes the property of that the alkoxy phenol of guaiacol, etc. and alkaline earth metal can be used to produce insoluble salt, and can be separated from other phenols.

The third is the sodium salt method, which has the reaction formula:

the natural guaiacol sodium salt is obtained by filtering, washing, acid precipitation, re-washing and rectification.

The fourth is the potassium salt process, which has the formula:

the natural guaiacol potassium salt is obtained by filtering, washing, acid precipitation, re-washing and rectification.

The third and fourth methods are to separate the alkoxyphenol such as natural guaiacol from other monophenol by utilizing the characteristic that the alkoxyphenol can generate crystalline solid with sodium hydroxide and potassium hydroxide solution.

Figure 1 is a block diagram of a process for extracting natural guaiacol. Now, the calcium salt method is taken as an example to explain the extraction of the natural guaiacol in detail. The first step is extraction, the forest miscellaneous phenol containing guaiacol is pumped into a stainless steel reaction kettle, then 10% sodium hydroxide is added, after the two are fully and evenly stirred, 20% calcium acetate solution is added while stirring. The dosage of the three raw materials is 2 parts, 6 parts and 3 parts by weight respectively according to the sequence of adding materials. The second step is filtration, and after the extract is cooled and crystallized, the upper mother liquor is extracted. The third procedure is to discharge clean water to wash the sediment twice and pump out the washing water. The fourth procedure is acid precipitation, sulfuric acid with the concentration adjusted to 30% is added from the elevated tank and fully stirred, the crude guaiacol gradually floats on the upper layer, after the acid precipitation is finished, sulfate wastewater is discharged from the bottom, and then the crude guaiacol is washed twice by clean water.

The four working procedures are all carried out in the same stainless steel reaction kettle. And if the three raw and auxiliary materials and the weight parts in the first process are taken as the reference, the consumption of 30 percent sulfuric acid in the fourth process is 2.84 parts. And the fifth procedure is decompression rectification, the crude guaiacolafter washing is pumped into a stainless steel rectification kettle, the vacuum degree in the kettle is controlled to be 0.082-0.083 MPa, the temperature in the kettle is controlled by heating equipment, and the fraction within the range of 148-151 ℃ is collected, namely the natural guaiacol. If the vacuum in the kettle is different, the temperature of the collected fraction is changed correspondingly.

The raw and auxiliary materials of the guaiacol synthesized in China at present are sodium nitrite, anthranilate and sulfuric acid, and the anthranilate is obtained by converting imported o-nitrochlorobenzene by a special factory.

By adopting the process for extracting the natural guaiacol, raw and auxiliary materials are all taken from China, foreign exchange is saved, and the purity of the obtained natural guaiacol is two percent higher than that of the domestic synthetic guaiacol and can reach 97 percent. The prior impure phenol discharged into rivers finds a new way, not only reduces the environmental pollution, but also increases the economic income, the extraction rate of the natural guaiacol reaches more than 60 percent, and the production cost is about 30 percent lower than that of the synthetic method. Vanillin produced with natural guaiacol is of much better quality than vanillin produced with synthetic guaiacol.

The best embodiment of the invention is as follows: 100 kg of lignified heterophenol containing 26% of guaiacol, 300 kg of sodium hydroxide solution containing 10%, 150 kg of calcium acetate solution containing 20% and 122 kg of sulfuric acid containing 30%, namely 2 parts, 6 parts, 3 parts and 2.84 parts of the required four raw and auxiliary materials by weight are carried out according to the process steps and the technical conditions in the specification to obtain 18 kg of natural guaiacol with the content of 95%, and the extraction rate is 69.23%.

Claims

1. The method for extracting the natural guaiacol from the forest chemical impure phenol is characterized by comprising the following steps: the first step is extraction, the forest miscellaneous phenols containing guaiacol is pumped into a stainless steel reaction kettle, and then sodium hydroxide with the concentration of 10% is added to fully and uniformly stir the two. The second step is filtration, and after the extract is cooled and crystallized, the upper mother liquor is extracted. The third procedure is to discharge clean water for washing and pump out the washing water. The fourth procedure is acid precipitation, sulfuric acid with the concentration adjusted to 30% is added and fully stirred, after the acid precipitation is finished, sulfate wastewater is discharged from the bottom, and then the crude guaiacol is washed by clean water. The four working procedures are carried out in the same stainless steel reaction kettle. And the fifth procedure is decompression rectification, wherein the crude guaiacol after washing is pumped into a stainless steel rectifying still, the rectifying still is heated by heating equipment, and the vacuum degree in the rectifying still corresponds to the temperature of the collected natural guaiacol one by one.

2. The method of claim 1 for extracting natural guaiacol from linza phenols, comprising the steps of: in the first step, 10% sodium hydroxide is added, and 10% potassium hydroxide can be added instead.

3. The process of claim 1 for extracting guaiacol from linza phenol, wherein: in the first procedure, the two materials are fully and uniformly stirred, and then the calcium acetate solution with the concentration of 20% is added while stirring, and the dosage of the three raw materials and the auxiliary materials isrespectively 2 parts, 6 parts and 3 parts by weight according to the adding sequence of the materials.

4. The method of claim 1 for extracting natural guaiacol from linza phenols, comprising the steps of: in the first step, the magnesium acetate solution is added while stirring after the magnesium acetate solution and the magnesium acetate solution are fully stirred.

5. The process for extracting natural guaiacol from linza phenols as claimed in claim 1 or 2, wherein: and a fifth step of controlling the vacuum degree in the kettle to be 0.082-0.083 MPa and collecting the fraction with the temperature in the kettle ranging from 148 ℃ to 151 ℃.

6. The method of claim 3 for extracting natural guaiacol from linza phenols, wherein: and a fifth step of controlling the vacuum degree in the kettle to be between 0.082 and 0.083MPa and collecting the fraction with the temperature in the kettle being between 148 and 151 ℃.

7. The method of claim 4 for extracting natural guaiacol from linoded fusel, wherein: and a fifth step of controlling the vacuum degree in the kettle to be between 0.082 and 0.083MPa and collecting the fraction with the temperature in the kettle being between 148 and 151 ℃.

8. The method of claim 6 for extracting natural guaiacol from linza phenols, wherein: the amount of the sulfuric acid with the concentration of 30 percent in the fourth working procedure is 2.84 parts by weight. And a fifth step of collecting a fraction having an internal temperature of 149 to 150 ℃.