CN102432428A - Method for purifying chromatographically pure organic solvent tert-butyl alcohol - Google Patents
Method for purifying chromatographically pure organic solvent tert-butyl alcohol Download PDFInfo
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- CN102432428A CN102432428A CN2011104409540A CN201110440954A CN102432428A CN 102432428 A CN102432428 A CN 102432428A CN 2011104409540 A CN2011104409540 A CN 2011104409540A CN 201110440954 A CN201110440954 A CN 201110440954A CN 102432428 A CN102432428 A CN 102432428A
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- trimethyl carbinol
- organic solvent
- chromatographically pure
- pure organic
- purification process
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Abstract
The invention relates to a method for purifying chromatographically pure organic solvent tert-butyl alcohol, which comprises the following steps: passing the raw material tert-butyl alcohol through 4A molecular sieves to remove a small quantity of organic impurities and water, drying, rectifying with calcium hydride, and packaging the effluent liquid, thereby obtaining the high performance liquid chromatography (HPLC) tert-butyl alcohol product. The invention can obtain the chromatographic tert-butyl alcohol product, of which the purity is greater than 99.9%, the yield is greater than 94% and the qualification rate is greater than 94%; and the invention can satisfy the application demands of users of HPLC reagent tert-butyl alcohol in the aspects of scientific experimentation, subject study and the like. Meanwhile, compared with the conventional method, the invention has the advantages of high product purity and stable product quality, and is simple to operate and suitable for large-scale production.
Description
Technical field:
The invention belongs to chemical technology field, relate to the purification process of organic solvent, especially a kind of purification process of the chromatographically pure organic solvent trimethyl carbinol.
Background technology:
The trimethyl carbinol is widely used as aspects such as solvent, additive, synthetic drugs, the high-purity iso-butylene of manufacturing and scientific research and testing.
Because commercially available trimethyl carbinol reagent contains moisture and various alcohols, its content is about about 99%.This kind trimethyl carbinol can not satisfy the needs of related science research trial, must be through being further purified, and making its each item technical indicator all reach chromatographic grade standard could use.
At present, domestic data about trimethyl carbinol purifying aspect mainly is that general method is difficult to impurity is removed, and therefore, the present invention is directed to this technical barrier and proposes effective solution because few through the content of impurity in the trimethyl carbinol of preliminary purification seldom.
Summary of the invention:
The objective of the invention is to overcome the deficiency of prior art, the purification process of the chromatographically pure organic solvent trimethyl carbinol that a kind of technology is simple, impurity is easily separated, product purity is high is provided.
The present invention is through following scheme implementation:
A kind of purification process of the chromatographically pure organic solvent trimethyl carbinol, step is following:
(1) flow velocity of the adsorption column of the raw material trimethyl carbinol through sorbent material is housed with 30mL-80mL/min carried out
Absorption;
(2) trimethyl carbinol after will adsorbing carries out drying through the dry post that siccative is housed, and dried water cut is controlled at≤and 0.05%;
(3) the dried trimethyl carbinol is squeezed into rectifying still and carry out rectifying, temperature is 120 ℃～200 ℃ at the bottom of the rectifying still, and fluid temperature is 100 ℃～120 ℃ in the still, and still top temperature is 82 ℃～83 ℃, total reflux 2～3 hours, control reflux ratio 1: 0.5～6.Filtering with microporous membrane after the rectifying, filtrating is the chromatographic grade trimethyl carbinol.
And sorbent material is the 4A molecular sieve in the described step (1), and the aperture is 4A.
And the material purity in the described step (1) is about 99%.
And siccative is hydrolith or Anhydrous potassium carbonate in the described step (2).
And warp was dry before siccative hydrolith or Anhydrous potassium carbonate used in the described step (2).
And, in said step (1) and (2) dress post amount be post high 4/5.
And the specification of said dry post is identical with adsorption column.
And the flow velocity of the trimethyl carbinol is 40mL-80mL/min in the described step (2).
Advantage of the present invention and positively effect are:
1, the present invention is about 99% the trimethyl carbinol with content and is raw material, carries out adsorption dry with the 4A molecular sieve as adsorption desiccant; Separate and remove impurity and moisture wherein; Adopt hydrolith or Anhydrous potassium carbonate further to remove moisture wherein as siccative; Process adsorption dry, rectifying purifying obtain the trimethyl carbinol product of purity 99.9%, and all other chromatogram indexs all reach requirement.
2, this preparation method yield rate is increased to more than 90% by 70%, and method is simple, and impurity is easily separated, and product purity is high, and is stable, saved manpower, reduced the consumption of the energy, more is applicable to industrialized production and application, has remarkable economic efficiency.
3, the product recovery rate of this preparation method production is greater than 94%, and yield rate reaches 94%, and this product can satisfy the user of performance liquid chromatography (HPLC) in scientific experiment, subject study and the application demand aspect other.
Embodiment:
Through specific embodiment the present invention is made further detailed description below, following examples are descriptive,
Not determinate, can not limit protection scope of the present invention with this.
Embodiment 1:
A kind of purification process of the chromatographically pure organic solvent trimethyl carbinol, step is following:
(1) the raw material trimethyl carbinol (content is about 99%) is promoted to adsorption column top, the high 1.8M of adsorption column, diameter 6.0cm, interior dress 4A molecular sieve (with preceding in 350 ℃ of activation) sorbent material, adorn the post amount and be post high 4/5, raw material carries out adsorption-edulcoration with 30mL/min speed;
In this step, the trimethyl carbinol fully contacts with the 4A molecular sieve in the adsorption column, removes impurity such as alcohols and water, detects the fluid quality and gets into next-step operation, and remove the high absorption front-end volatiles of impurity near qualified (concrete technical indicator is seen table 1) back.
(2) effluent in the step (1) is got into dry post, the specification of dry post, the same adsorption column of dress post amount are packed in the post through the exsiccant hydrolith, and flow velocity is about 40mL/min.Detect dried trimethyl carbinol water cut, moisture controlled is≤0.05%;
Moisture content＞0.05% o'clock utilize hydrolith to remove the moisture in the trimethyl carbinol after adsorbing in this step, if carry out drying treatment after needing to change siccative again.
(3) with getting into rectifying still through the dried trimethyl carbinol in the step (2), the amount that adds hydrolith in the still is 0.2～2% of a raw material.Carry out rectifying, utilize electrically heated, temperature is about 120 ℃ at the bottom of the rectifying still, and fluid temperature is 100 ℃ in the still, and rectifying goes out 82 ℃～83 ℃ of liquid temps, and control reflux ratio 1: 0.5～2 refluxed 1～1.5 hour.Remove front-end volatiles, the qualified after 0.45 μ mNYL filtering with microporous membrane of distillate, bottling seals under nitrogen protection, promptly gets the chromatographic grade trimethyl carbinol that meets index request;
Greater than 99.9%, its front-end volatiles are for further processing through its purity of check.
Embodiment 2:
A kind of purification process of the chromatographically pure organic solvent trimethyl carbinol, step is following:
(1) the raw material trimethyl carbinol (content is 99%) is promoted to adsorption column top, the high 1.8M of adsorption column, diameter 6.0cm, interior dress 4A molecular sieve (with preceding in 350 ℃ of activation) sorbent material, adorn the post amount and be post high 4/5, raw material carries out adsorption-edulcoration with 80mL/min speed;
In this step, the trimethyl carbinol fully contacts with the 4A molecular sieve in the adsorption column, removes impurity such as alcohols and water, detects the fluid quality and gets into next-step operation, and remove the high absorption front-end volatiles of impurity near qualified (concrete technical indicator is seen table 1) back.
(2) effluent in the step (1) is got into dry post, the specification of dry post, the same adsorption column of dress post amount are packed in the post through baking exsiccant Anhydrous potassium carbonate, and flow velocity is 80mL/min.Detect dried trimethyl carbinol water cut, moisture controlled is≤0.05%;
Moisture content＞0.05% o'clock utilize Anhydrous potassium carbonate to remove the moisture in the trimethyl carbinol after adsorbing in this step, if carry out drying treatment after needing to change siccative again.
(3) with getting into rectifying still through the dried trimethyl carbinol in the step (2), the amount that adds hydrolith in the still is 3～5% of a raw material.Carry out rectifying, utilize electrically heated, temperature is about 200 ℃ at the bottom of the rectifying still, and fluid temperature is 120 ℃ in the still, and rectifying goes out 82 ℃～83 ℃ of liquid temps, control reflux ratio 1: 3～6, and 2～3 hours fluids reflux.Remove front-end volatiles, the qualified after 0.45 μ mNYL filtering with microporous membrane of distillate, bottling seals under nitrogen protection, promptly gets the chromatographic grade trimethyl carbinol that meets index request;
Greater than 99.9%, its front-end volatiles are for further processing through its purity of check.
Effect detection:
The purified high-purity organic solvent trimethyl carbinol is in ultraviolet wavelength 215nm～400nm scope (the quartzy cuvette of 1cm, water is made reference); Absorbancy satisfies the index request in the table 1; Content is greater than 99.9%, moisture≤0.05%, and the recovery is greater than 94%; Yield rate reaches more than 94% approximately, and all other indexs meet the requirements.
Table 1: the technical indicator of raw material, the chromatographically pure trimethyl carbinol
Claims (8)
1. the purification process of a chromatographically pure organic solvent trimethyl carbinol, it is characterized in that: step is following:
(1) flow velocity of the adsorption column of the raw material trimethyl carbinol through sorbent material is housed with 30mL-80mL/min adsorbed;
(2) trimethyl carbinol after will adsorbing carries out drying through the dry post that siccative is housed, and dried water cut is controlled at≤and 0.05%;
(3) the dried trimethyl carbinol is squeezed into rectifying still and carry out rectifying, temperature is 120 ℃～200 ℃ at the bottom of the rectifying still, and fluid temperature is 100 ℃～120 ℃ in the still, and still top temperature is 82 ℃～83 ℃, total reflux 2～3 hours, control reflux ratio 1: 0.5～6.Filtering with microporous membrane after the rectifying, filtrating is the chromatographic grade trimethyl carbinol.
2. the purification process of a kind of chromatographically pure organic solvent trimethyl carbinol according to claim 1 is characterized in that: sorbent material is the 4A molecular sieve in the described step (1), and the aperture is 4A.
3. the purification process of a kind of chromatographically pure organic solvent trimethyl carbinol according to claim 1 is characterized in that: the material purity in the described step (1) is about 99%.
4. the purification process of a kind of chromatographically pure organic solvent trimethyl carbinol according to claim 1 is characterized in that: siccative is hydrolith or Anhydrous potassium carbonate in the described step (2).
5. the purification process of a kind of chromatographically pure organic solvent trimethyl carbinol according to claim 4 is characterized in that: warp was dry before siccative hydrolith or Anhydrous potassium carbonate used in the described step (2).
6. the purification process of a kind of chromatographically pure organic solvent trimethyl carbinol according to claim 1 is characterized in that: in said step (1) and (2) dress post amount be post high 4/5.
7. the purification process of a kind of chromatographically pure organic solvent trimethyl carbinol according to claim 1 is characterized in that: the specification of said dry post is identical with adsorption column.
8. the purification process of a kind of chromatographically pure organic solvent trimethyl carbinol according to claim 1 is characterized in that: the flow velocity of the trimethyl carbinol is 40mL-80mL/min in the described step (2).
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011104409540A CN102432428A (en) | 2011-12-26 | 2011-12-26 | Method for purifying chromatographically pure organic solvent tert-butyl alcohol |
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| CN2011104409540A CN102432428A (en) | 2011-12-26 | 2011-12-26 | Method for purifying chromatographically pure organic solvent tert-butyl alcohol |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731251A (en) * | 2012-07-06 | 2012-10-17 | 天津市康科德科技有限公司 | Purification method of highly pure organic solvent n-butanol |
| CN107324972A (en) * | 2017-08-29 | 2017-11-07 | 湖北工程学院 | A kind of chromatographically pure tert-butyl alcohol and preparation method thereof, production system |
| CN107382669A (en) * | 2017-08-29 | 2017-11-24 | 湖北工程学院 | Chromatographically pure n-butanol and preparation method thereof, production system |
| CN108083973A (en) * | 2016-11-21 | 2018-05-29 | 国药集团化学试剂有限公司 | A kind of purification process of tetrachloro-ethylene |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1860090A (en) * | 2003-10-17 | 2006-11-08 | 利安德化学技术有限公司 | Purification of tertiary butyl alcohol |
| CN102060663A (en) * | 2009-11-18 | 2011-05-18 | 天津市康科德科技有限公司 | Method for preparing chromatographic pure isopropanol |
-
2011
- 2011-12-26 CN CN2011104409540A patent/CN102432428A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1860090A (en) * | 2003-10-17 | 2006-11-08 | 利安德化学技术有限公司 | Purification of tertiary butyl alcohol |
| CN102060663A (en) * | 2009-11-18 | 2011-05-18 | 天津市康科德科技有限公司 | Method for preparing chromatographic pure isopropanol |
Non-Patent Citations (1)
| Title |
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| 许春建，吕东来: "吸附蒸馏提纯叔丁醇及异丙醇", 《化学工业与工程》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731251A (en) * | 2012-07-06 | 2012-10-17 | 天津市康科德科技有限公司 | Purification method of highly pure organic solvent n-butanol |
| CN102731251B (en) * | 2012-07-06 | 2014-07-02 | 天津康科德医药化工有限公司 | Purification method of highly pure organic solvent n-butanol |
| CN108083973A (en) * | 2016-11-21 | 2018-05-29 | 国药集团化学试剂有限公司 | A kind of purification process of tetrachloro-ethylene |
| CN107324972A (en) * | 2017-08-29 | 2017-11-07 | 湖北工程学院 | A kind of chromatographically pure tert-butyl alcohol and preparation method thereof, production system |
| CN107382669A (en) * | 2017-08-29 | 2017-11-24 | 湖北工程学院 | Chromatographically pure n-butanol and preparation method thereof, production system |
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Application publication date: 20120502 |