CN1119307C - New extracting method for natural guaiacol - Google Patents
New extracting method for natural guaiacol Download PDFInfo
- Publication number
- CN1119307C CN1119307C CN00101301A CN00101301A CN1119307C CN 1119307 C CN1119307 C CN 1119307C CN 00101301 A CN00101301 A CN 00101301A CN 00101301 A CN00101301 A CN 00101301A CN 1119307 C CN1119307 C CN 1119307C
- Authority
- CN
- China
- Prior art keywords
- methyl catechol
- guaiacol
- fraction
- creosote
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
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- LHGVFZTZFXWLCP-UHFFFAOYSA-N guaiacol Chemical compound COC1=CC=CC=C1O LHGVFZTZFXWLCP-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229960001867 guaiacol Drugs 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 17
- WHRZCXAVMTUTDD-UHFFFAOYSA-N 1h-furo[2,3-d]pyrimidin-2-one Chemical compound N1C(=O)N=C2OC=CC2=C1 WHRZCXAVMTUTDD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 235000006173 Larrea tridentata Nutrition 0.000 claims abstract description 9
- 244000073231 Larrea tridentata Species 0.000 claims abstract description 9
- 229960002126 creosote Drugs 0.000 claims abstract description 9
- 238000000605 extraction Methods 0.000 claims abstract description 7
- 238000007710 freezing Methods 0.000 claims abstract description 7
- 230000008014 freezing Effects 0.000 claims abstract description 7
- 239000000284 extract Substances 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000002253 acid Substances 0.000 abstract description 2
- 238000005235 decoking Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000004821 distillation Methods 0.000 abstract 3
- 230000002349 favourable effect Effects 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 238000010189 synthetic method Methods 0.000 abstract 1
- 238000005119 centrifugation Methods 0.000 description 3
- 238000005194 fractionation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000010923 batch production Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011020 pilot scale process Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A new method for extracting natural guaiacol from silvichemical creosote only needs three main procedures of distillation, freezing and centrifugal separation, which is simpler than the existing domestic synthetic methods or the procedures of insoluble salt production, filtration, acid out, decoking, rough distillation and refined distillation. Moreover, the method has the advantages of low production cost, high extraction rate of guaiacol, high purity, and favorable social and economic benefits; the method is suitable for industrial production.
Description
The methyl catechol purity that the production of present domestic employing synthesis technique obtains is lower; The extraction of natural guaiacol, the patent No. is 9310220 patent of invention, to pass through filtration, acid out, decoking, slightly heat up in a steamer, operation such as rectifying, the methyl catechol purity that obtains is the highest can only to reach 95%, this processes expend raw and auxiliary material, extraction yield is not high, and the production cost height is difficult to change into productivity.
In order from the woodsization creosote, to extract highly purified methyl catechol, simplify extraction process, reduce production costs, improve the extraction yield of methyl catechol, the contriver found out a cover in recent years and extracted the novel process of natural guaiacol, and had carried out pilot scale and batch process.
From the woodsization creosote, extract the method for natural guaiacol, its technological process in the following order: rectifying, freezing, centrifugation obtain the methyl catechol product, see Fig. 1.When the woodsization creosote suction stainless steel rectifying still that will contain methyl catechol 20～30%, heat temperature raising to 100 ℃, start vacuum pump, withdrawing moisture and light fraction after moisture content and light fraction have extracted, obtain methyl catechol content greater than 50% fraction with rectifying; The fraction that second step will be contained greater than 50% methyl catechol enters freezer, and the temperature in freezer room is controlled between 0～-20 ℃, and freezing time is 12～48 hours, allows methyl catechol separate out crystallization in this humidity province; Three-procedure is centrifugation, the methyl catechol work in-process of separating out in the freezer room is sent into whizzer carry out separating treatment, and the methyl catechol that centrifugation obtains is dissolved into oily matter at normal temperatures, obtains purity and reaches 99% natural guaiacol product.
Most preferred embodiment of the present invention: the woodsization creosote 3000kg suction capacity that will contain 28% methyl catechol is in 4 cubic metres the rectifying still, be warming up to 100 ℃, open vacuum pump, extract moisture content and light fraction, when the temperature in the rectifying still was raised to 130 ℃, light fraction extracted and finishes; Temperature in the kettle is since 130 ℃, transfer fractionation methyl catechol fraction section to, when temperature in the kettle arrives 140 ℃, fractionation methyl catechol fraction finishes, this moment, methyl catechol content was up to 50～85%, subsequently the methyl catechol fraction sent into-10 ℃ freezing 24 hours of freezer, and the methyl catechol crystal of separating out separates with whizzer, obtain 673kg purity and be 99% natural guaiacol, extraction yield is 80%.
The present invention extracts the method for natural guaiacol from the woodsization creosote need not pass through chemical treatment, does not consume raw and auxiliary material, and technology is easy to be reliable, the yield height, and the product purity height, production cost is low, and very suitability for industrialized production has good social benefit and economic benefit.
Claims (2)
1, from the woodsization creosote, extracts the method for natural guaiacol: it is characterized in that, the woodsization creosote suction stainless steel rectifying still that will contain methyl catechol 20～30%, during heat temperature raising to 100 ℃, start vacuum pump, withdrawing moisture and light fraction, after moisture content and light fraction have extracted, with the temperature in the rectifying still be controlled at 130～140 ℃, when vacuum pressure is controlled at 0.08～0.09Mpa, rectifying this moment obtains methyl catechol content greater than 50% fraction; Second step will be contained greater than the fraction of 50% methyl catechol and send into freezer, and the temperature in freezer room is controlled between 0～-20 ℃, and freezing time is 12～48 hours, allows methyl catechol separate out crystallization in this humidity province; The 3rd step will be separated out the crystalline methyl catechol and be sent into whizzer and separate and obtain the methyl catechol crystal in the freezer room;
By the method for the described extraction natural guaiacol of claim 1, it is characterized in that 2, the freezing temperature that contains greater than 50% methyl catechol is-10 ℃, freezing time is 24 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00101301A CN1119307C (en) | 2000-01-01 | 2000-01-01 | New extracting method for natural guaiacol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00101301A CN1119307C (en) | 2000-01-01 | 2000-01-01 | New extracting method for natural guaiacol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1270949A CN1270949A (en) | 2000-10-25 |
| CN1119307C true CN1119307C (en) | 2003-08-27 |
Family
ID=4575864
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN00101301A Expired - Fee Related CN1119307C (en) | 2000-01-01 | 2000-01-01 | New extracting method for natural guaiacol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1119307C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111499499B (en) * | 2020-04-03 | 2023-12-22 | 上海道沌机械设备有限公司 | Purification method and purification system of natural guaiacol |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1040744A (en) * | 1988-08-29 | 1990-03-28 | 唐化学原料公司 | Hydrogen Sulfide Removal from Fluid Streams |
-
2000
- 2000-01-01 CN CN00101301A patent/CN1119307C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1040744A (en) * | 1988-08-29 | 1990-03-28 | 唐化学原料公司 | Hydrogen Sulfide Removal from Fluid Streams |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1270949A (en) | 2000-10-25 |
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