CN101704725B - Purification method of dinonylphenol - Google Patents
Purification method of dinonylphenol Download PDFInfo
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- CN101704725B CN101704725B CN2009102125937A CN200910212593A CN101704725B CN 101704725 B CN101704725 B CN 101704725B CN 2009102125937 A CN2009102125937 A CN 2009102125937A CN 200910212593 A CN200910212593 A CN 200910212593A CN 101704725 B CN101704725 B CN 101704725B
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- binonylphenol
- dinonylphenol
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Abstract
The invention discloses a purification method of dinonylphenol. The purification method comprises the following steps: firstly collecting residual dinonylphenol in nonyl phenol as initial extract, using a vacuum pump to absorb the initial extract into a batch-type distillation still, then increasing the temperature of the distillation still to 190 DEG C to 210 DEG C, and heating for 1.5 to 2.5 hours under the state that the vacuum degree is 0.7 to 0.9kPa; then adding a stabilizer N, N-diethylhydroxylamine with the weight of 0.9 to 1.1 per thousand of that of the initial extract, continuously reacting for 4 to 6 minutes, increasing the temperature of the distillation still to 250 DEG C, then starting to produce a dinonylphenol pure product till the distillation is finished. The content of the dinonylphenol produced by the invention is about 80 percent, and compared with the products of other domestic manufacturers, the purity thereof is greatly improved. When the used amount of the initial extract is eight tons, the whole distillation process needs about 12 hours, and the obtained high-purity dinonylphenol is about 85 to 90 percent of the total amount of the used dinonylphenol.
Description
Technical field
The present invention relates to a kind of chemical purification method of material, specifically is a kind ofly will produce the method that the binonylphenol that produces in the NP process is purified.
Background technology
In chemical field, NP is a kind of important fine chemical material and midbody, and outward appearance is colourless or weak yellow liquid at normal temperatures, has a little the phenol smell, and is water insoluble, is dissolved in acetone.It is mainly used in and produces tensio-active agent, also is used for oxidation inhibitor, textile auxiliary, oil dope, farm chemical emulgent, modifier, resin and rubber stablizer.The working method of NP is with phenol and nonene reacted NP; In this process, can produce a large amount of by product---binonylphenols; Conventional art does not reclaim these binonylphenols, if these binonylphenols can not get using, will cause great resource wave.The applicant once proposed one binonylphenol was converted to the patent of invention of NP, in order better to realize this conversion, need collect earlier and the production process of withdrawing deposit in the binonylphenol that produces.And in the producer of present domestic existing production NP, also do not produce the binonylphenol that produces in the NP process to extract the content that perhaps extracts yet not high (probably about 20%).
Summary of the invention
Technical problem to be solved by this invention provides a kind of by product to being produced in the NP production process---the method that binonylphenol is purified, and the binonylphenol content that this method is purified is high, and the time of withdrawing deposit is short, less energy consumption.
The method of purification of binonylphenol of the present invention; May further comprise the steps: at first collect binonylphenol residual in the NP as primary extract; Utilize vacuum pump that primary extract is sucked the batch distillation still; Make the still kettle temperature rise to 190-210 ℃ again, vacuum tightness for the 0.7-0.9kPa state under the heating 1.5-2.5 hour; The stablizer N that adds 0.9-1.1 ‰ primary extract weight then, the N-diethyl hydroxylamine continued reaction after 4-6 minute, and the temperature of still kettle is risen to 250 ℃, began the pure article of output binonylphenol subsequently, finished up to distillation.
The binonylphenol content of output of the present invention about 80%, the product of domestic relatively other producer, its purity improves greatly.At the primary extract consumption is 8 ton hours, and whole still-process approximately needs 12 hours, and gained high purity binonylphenol is approximately and drops into 85%～90% of binonylphenol total amount.
Embodiment
Below in conjunction with specific embodiment the present invention is set forth.
Embodiment 1:
In the DCS automatic production, collect the residual binonylphenol in the NP, collect 8 ton hours when binonylphenol, utilize vacuum pump that binonylphenol is sucked the batch distillation still; Utilizing the outer circulation heating again, the still kettle temperature is risen to about 190 ℃, is under the 0.7kPa state in vacuum tightness; Heated 1.5 hours, and added the stablizer N of 7.2kg then, (ten thousand longevity of Wujin chemical plant produces the N-diethyl hydroxylamine; Content 97%), after 4 minutes, the temperature of still kettle is risen to 250 ℃; Soon just begin the binonylphenol of output content about 80%, whole still-process approximately needs 12 hours, and gained high purity binonylphenol is approximately and drops into 85%～90% of binonylphenol total amount.
Embodiment 2:
In the DCS automatic production, collect the residual binonylphenol in the NP, when binonylphenol is collected 8 tons of left and right sides; Utilize vacuum pump that binonylphenol is sucked the batch distillation still, utilize the outer circulation heating again, the still kettle temperature is risen to about 210 ℃; In vacuum tightness is under the 0.9kPa state, heats 2.5 hours, adds the stablizer N of 8.8kg then; N-diethyl hydroxylamine (ten thousand longevity of Wujin chemical plant produces, content 97%) is after 6 minutes; The temperature of still kettle is risen to 250 ℃; Soon just begin the binonylphenol of output content about 80%, whole still-process approximately needs 12 hours, and gained high purity binonylphenol is approximately and drops into 85%～90% of binonylphenol total amount.
Embodiment 3:
In the DCS automatic production, collect the residual binonylphenol in the NP, collect 8 ton hours when binonylphenol, utilize vacuum pump that binonylphenol is sucked the batch distillation still; Utilizing the outer circulation heating again, the still kettle temperature is risen to about 200 ℃, is under the 0.8kPa state in vacuum tightness; Heated 2 hours, and added the stablizer N of 8kg then, (ten thousand longevity of Wujin chemical plant produces the N-diethyl hydroxylamine; Content 97%), after 5 minutes, the temperature of still kettle is risen to 250 ℃; Soon just begin the binonylphenol of output content about 80%, whole still-process approximately needs 12 hours, and gained high purity binonylphenol is approximately and drops into 85%～90% of binonylphenol total amount.
Table 1 is each item index of residual binonylphenol in the NP before withdrawing deposit, and table 2 is to adopt the product that the present invention purifies and the contrast of other producer's refined product.
Subordinate list one: each item index of residual binonylphenol in the NP
| Colourity (Pt-Co) | Content | Moisture content | Hydroxyl value | Phenol | Other alkylphenol | |
| Binonylphenol | 70 | 30％ | 0.07％ | 245~255 | 0.06％ | 70％ |
Subordinate list two: the binonylphenol of the present invention and other plant produced (back of purifying) each item index contrast
Claims (2)
1. the method for purification of a binonylphenol; It is characterized in that may further comprise the steps: at first collect binonylphenol residual in the NP as primary extract; Utilize vacuum pump that primary extract is sucked the batch distillation still; Make the still kettle temperature rise to 190-210 ℃ again, vacuum tightness for the 0.7-0.9kPa state under the heating 1.5-2.5 hour; The stablizer N that adds 0.9-1.1 ‰ primary extract weight then, the N-diethyl hydroxylamine continued reaction after 4-6 minute, and the temperature of still kettle is risen to 250 ℃, began the pure article of output binonylphenol subsequently, finished up to distillation.
2. the method for purification of binonylphenol according to claim 1 is characterized in that utilizing the outer circulation type of heating to improve the batch distillation temperature in the kettle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102125937A CN101704725B (en) | 2009-11-12 | 2009-11-12 | Purification method of dinonylphenol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102125937A CN101704725B (en) | 2009-11-12 | 2009-11-12 | Purification method of dinonylphenol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101704725A CN101704725A (en) | 2010-05-12 |
| CN101704725B true CN101704725B (en) | 2012-05-23 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2009102125937A Active CN101704725B (en) | 2009-11-12 | 2009-11-12 | Purification method of dinonylphenol |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100486947C (en) * | 2005-11-23 | 2009-05-13 | 中国石油天然气集团公司 | Nonyl phenol refining process |
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2009
- 2009-11-12 CN CN2009102125937A patent/CN101704725B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100486947C (en) * | 2005-11-23 | 2009-05-13 | 中国石油天然气集团公司 | Nonyl phenol refining process |
Non-Patent Citations (1)
| Title |
|---|
| 岳丽娟等.壬基酚产品变色原因和控制途径探讨.《黑龙江石油化工》.2000,第11卷 * |
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| CN101704725A (en) | 2010-05-12 |
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Address after: 214264 Fang Qiao Industrial Park, Jiangsu, Yixing Applicant after: Jiangsu Lingfei Technology Co.,Ltd. Address before: 214264 Fang Qiao Industrial Park, Jiangsu, Yixing Applicant before: Jiangsu Lingfei Chemical Co., Ltd. |
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Free format text: CORRECT: APPLICANT; FROM: JIANGSU LINGFEI CHEMICAL CO., LTD. TO: JIANGSU LINGFEI TECHNOLOGY CO., LTD. |
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Effective date of registration: 20210622 Address after: No. 11, Zha Nan Road, Taixing Economic Development Zone, Taizhou City, Jiangsu Province 225442 Patentee after: TAIXING LINGFEI CHEMICAL TECHNOLOGY Co.,Ltd. Address before: 214264 Fangqiao Industrial Park, Yixing City, Jiangsu Province Patentee before: JIANGSU LINGFEI TECHNOLOGY Co.,Ltd. |