CN102417434A - Method for purifying chromatographic grade organic solvent carbon tetrachloride - Google Patents
Method for purifying chromatographic grade organic solvent carbon tetrachloride Download PDFInfo
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- CN102417434A CN102417434A CN2011104409517A CN201110440951A CN102417434A CN 102417434 A CN102417434 A CN 102417434A CN 2011104409517 A CN2011104409517 A CN 2011104409517A CN 201110440951 A CN201110440951 A CN 201110440951A CN 102417434 A CN102417434 A CN 102417434A
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- tetracol phenixin
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Abstract
The invention relates to a method for purifying a high-purity organic solvent carbon tetrachloride. The method comprises the following steps of: percolating a raw material, namely carbon tetrachloride by using a silicagel column so as to remove organic impurities, anhydrous calcium chloride or magnesium sulfate, drying and dehydrating, rectifying by using a rectifying still, filtering, and charging nitrogen and storing to obtain a high-purity organic solvent carbon tetrachloride product. By the method, a chromatographic grade carbon tetrachloride product with the purity of more than 99.9 percent can be obtained, the yield is over 94 percent, the qualification rate is over 95 percent, and application requirements of users of a high performance liquid chromatography (HPLC) reagent carbon tetrachloride on aspects such as scientific experiments, subject research and the like can be met; meanwhile, compared with the conventional method, the invention has the advantages that: the method is easy to operate and is suitable for large-scale production, and the product is high in purity and stable in quality.
Description
Technical field:
The invention belongs to chemical technology field, relate to the method for purification of organic solvent, especially a kind of method of purification of chromatographic grade organic solvent tetracol phenixin.
Background technology:
Tetracol phenixin is mainly used in the indentifying substance and the scientific research task experiment of organic synthesis, cooling agent, sterilant, pharmaceutical extraction, some metal and nonmetal and uses organic solvent.
The tetracol phenixin reagent of selling on the market, its content is about 99.5%, wherein contains impurity such as a small amount of dithiocarbonic anhydride, chloroform and water.This kind tetracol phenixin can not satisfy the needs of high-tech experimental study, must be through further purifying, and making its each item technical indicator all reach chromatographic grade standard can use.
At present, domestic data about tetracol phenixin purification aspect is reported seldom, mainly is owing to few through foreign matter content in the tetracol phenixin of preliminary purification, is difficult in the rectifying remove.Therefore, the present invention is directed to this technical barrier and propose effective solution.
Summary of the invention:
The objective of the invention is to overcome the deficiency of prior art, the method for purification of the chromatographic grade organic solvent tetracol phenixin 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 method of purification of chromatographic grade organic solvent tetracol phenixin, step is following:
(1) adsorption column of raw material tetracol phenixin through sorbent material is housed carried out diafiltration absorption with the flow velocity of 40mL～100mL/min;
(2) tetracol phenixin after will adsorbing carries out drying through the dry post that siccative is housed, and dried water cut is controlled at≤and 0.01%;
(3) dried tetracol phenixin is squeezed into rectifying still and carry out rectifying, temperature is 120～200 ℃ at the bottom of the rectifying still, and fluid temperature is 80 ℃～100 ℃ in the still, and still top temperature is 76 ℃～77 ℃, control reflux ratio 1: 0.5～9, and 2～3 hours fluids reflux.Filtering with microporous membrane after the rectifying, filtrating is the chromatographic grade tetracol phenixin.
And sorbent material is a silica gel in the described step (1), and granularity is 60 orders～100 orders.
And the material purity in the described step (1) is 99.5%.
And siccative is Calcium Chloride Powder Anhydrous or sal epsom in the described step (2).
And, dry before siccative Calcium Chloride Powder Anhydrous or sal epsom use in the described step (2) through baking.
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 tetracol phenixin is 80mL～120mL/min in the described step (2).
Advantage of the present invention and positively effect are:
1, the present invention is that 99.5% tetracol phenixin is raw material, carries out fractionation by adsorption with silica gel as the adsorptive percolation agent and remove impurity wherein with content; Adopt Calcium Chloride Powder Anhydrous or sal epsom to remove moisture wherein as siccative; Obtain purity greater than 99.9% tetracol phenixin product through absorption, dry, rectification and purification, all other chromatogram indexs all reach requirement.
2, this method of purification promotes carbon tetrachloride content to 99.9%; Yield rate is increased to more than 90% by original 65%; Method is simple, impurity is easily separated, product purity is high, stable, saving manpower; Reduce the consumption of the energy, more be applicable to industrialized production and application, have remarkable economic efficiency.
3, the product of this method of purification production is through detecting the requirement that its each item index meets the chromatographically pure tetracol phenixin; Its carbon tetrachloride content greater than 99.9%, the recovery greater than 94%, yield rate reaches 95%, can satisfy the application demand of the user of performance liquid chromatography (HPLC) at aspects such as scientific research task experiments.
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 method of purification of chromatographic grade organic solvent tetracol phenixin, step is following:
(1) raw material tetracol phenixin (content is 99.5%) is promoted to adsorption column top, the high 1.5M of adsorption column wherein, diameter 3.5cm, interior dress granularity 60 orders～80 purpose silica gel absorbers, dress post amount be post high 7/10, raw material carries out adsorption-edulcoration with 40mL/min speed;
In post; Tetracol phenixin fully contacts with silica gel absorber, removes impurity wherein through diafiltration absorption, detects the ultraviolet light absorption value of absorption fluid; It (is that effluent each item index is near chromatographic grade technical requirement that fluid to be adsorbed is up to the standards; Its concrete technical requirement is seen table 1) after, get into next-step operation, and remove the high absorption front-end volatiles of impurity.
(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 Calcium Chloride Powder Anhydrous, and flow velocity is 80mL/min.Detect dried tetracol phenixin water cut, moisture controlled is≤0.01%
Moisture content＞0.01% o'clock utilize Calcium Chloride Powder Anhydrous to remove the moisture in the tetracol phenixin after adsorbing in this step, if carry out drying treatment after needing to change siccative again.
(3) carry out rectifying with flowing into the glass rectifying still through dried tetracol phenixin in the step (2); Utilize electrically heated, temperature is about 120 ℃ at the bottom of the control still, and fluid temperature is 80 ℃ in the still; Going out liquid temp is 76～77 ℃; Total reflux 1.5～2 hours, the control reflux ratio went out front-end volatiles at 1: 0.5～1 o'clock, and the qualified back of fluid transfers reflux ratio 1: 4～5 to go out finished product.Finished product is behind 0.45 μ mPVDF filtering with microporous membrane, and the bottling sealing promptly gets the chromatographic grade tetracol phenixin product that meets index request under nitrogen protection.
Greater than 99.9%, its front-end volatiles are for further processing through its purity of check.
Embodiment 2:
A kind of method of purification of chromatographic grade organic solvent tetracol phenixin, step is following:
(1) raw material tetracol phenixin (content is 99.5%) is promoted to adsorption column top, the high 1.5M of adsorption column wherein, diameter 3.5cm, interior dress granularity 80 orders～100 purpose silica gel absorbers, dress post amount be post high 7/10, raw material carries out adsorption-edulcoration with 100mL/min speed;
In post; Tetracol phenixin fully contacts with silica gel absorber, removes impurity wherein through diafiltration absorption, detects the ultraviolet light absorption value of absorption fluid; It (is that effluent each item index is near chromatographic grade technical requirement that fluid to be adsorbed is up to the standards; Its concrete technical requirement is seen table 1) after, get into next-step operation, and remove the high absorption front-end volatiles of impurity.
(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 Calcium Chloride Powder Anhydrous, and flow velocity is 120mL/min.Detect dried tetracol phenixin water cut, moisture controlled is≤0.01%
Moisture content＞0.01% o'clock utilize anhydrous magnesium sulfate to remove the moisture in the tetracol phenixin after adsorbing in this step, if carry out drying treatment after needing to change siccative again.
(3) carry out rectifying with flowing into the glass rectifying still through dried tetracol phenixin in the step (2), utilize electrically heated, temperature is about 200 ℃ at the bottom of the control still; Fluid temperature is 100 ℃ in the still; Going out liquid temp is 76～77 ℃, total reflux 1.5～2 hours, and the control reflux ratio went out front-end volatiles at 1: 0.5～1 o'clock; The qualified back of fluid transfers reflux ratio 1: 5～9 to go out finished product; Finished product is behind 0.45 μ mPVDF filtering with microporous membrane, and the bottling sealing promptly gets the chromatographic grade tetracol phenixin product that meets index request under nitrogen protection.
Greater than 99.9%, its front-end volatiles are for further processing through its purity of check.
Effect detection:
High-purity organic solvent tetracol phenixin after the purification is in ultraviolet wavelength 265nm～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≤0.01%, and the recovery is greater than 94%; Yield rate reaches more than 95% approximately, and all other are the value of touching the mark all.
Table 1: the technical indicator of raw material, chromatographically pure tetracol phenixin
Claims (8)
1. the method for purification of a chromatographic grade organic solvent tetracol phenixin, it is characterized in that: step is following:
(1) adsorption column of raw material tetracol phenixin through sorbent material is housed carried out diafiltration absorption with the flow velocity of 40mL～100mL/min;
(2) tetracol phenixin after will adsorbing carries out drying through the dry post that siccative is housed, and dried water cut is controlled at≤and 0.01%;
(3) dried tetracol phenixin is squeezed into rectifying still and carry out rectifying, temperature is 120～200 ℃ at the bottom of the rectifying still, and fluid temperature is 80 ℃～100 ℃ in the still, and still top temperature is 76 ℃～77 ℃, control reflux ratio 1: 0.5～9, and 2～3 hours fluids reflux.Filtering with microporous membrane after the rectifying, filtrating is the chromatographic grade tetracol phenixin.
2. the method for purification of a kind of chromatographic grade organic solvent tetracol phenixin according to claim 1 is characterized in that: sorbent material is a silica gel in the described step (1), and granularity is 60 orders～100 orders.
3. the method for purification of a kind of chromatographic grade organic solvent tetracol phenixin according to claim 1 is characterized in that: the material purity in the described step (1) is 99.5%.
4. the method for purification of a kind of chromatographic grade organic solvent tetracol phenixin according to claim 1 is characterized in that: siccative is Calcium Chloride Powder Anhydrous or sal epsom in the described step (2).
5. the method for purification of a kind of chromatographic grade organic solvent tetracol phenixin according to claim 1 is characterized in that: dry through baking before siccative Calcium Chloride Powder Anhydrous or sal epsom use in the described step (2).
6. the method for purification of a kind of chromatographic grade organic solvent tetracol phenixin according to claim 1 is characterized in that: in said step (1) and (2) dress post amount be post high 4/5.
7. the method for purification of a kind of chromatographic grade organic solvent tetracol phenixin according to claim 1 is characterized in that: the specification of said dry post is identical with adsorption column.
8. the method for purification of a kind of chromatographic grade organic solvent tetracol phenixin according to claim 1 is characterized in that: the flow velocity of tetracol phenixin is 80mL～120mL/min in the described step (2).
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011104409517A CN102417434A (en) | 2011-12-26 | 2011-12-26 | Method for purifying chromatographic grade organic solvent carbon tetrachloride |
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| CN2011104409517A CN102417434A (en) | 2011-12-26 | 2011-12-26 | Method for purifying chromatographic grade organic solvent carbon tetrachloride |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105859510A (en) * | 2016-05-09 | 2016-08-17 | 江苏梅兰化工有限公司 | Continuous production process and device of high-purity carbon tetrachloride |
| CN106040206A (en) * | 2016-07-28 | 2016-10-26 | 王金明 | Preparation method of carbon tetrachloride purification adsorbent |
| CN106238009A (en) * | 2016-07-28 | 2016-12-21 | 王金明 | A kind of preparation method of carbon tetrachloride adsorbent |
| CN107353178A (en) * | 2017-06-26 | 2017-11-17 | 江苏南大光电材料股份有限公司 | The preparation method of ultra-pure carbon tetrachloride |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3631116A (en) * | 1968-01-12 | 1971-12-28 | Lothar Hornig | Process for the manufacture of carbon tetrachloride |
| CN1327952A (en) * | 2001-06-02 | 2001-12-26 | 吉林大学 | Equipment for purifying extractant of mineral oil in water and process for treating adsorbent |
| CN102093160A (en) * | 2010-12-29 | 2011-06-15 | 天津市康科德科技有限公司 | Method for preparing chromatographically-pure trichloromethane |
| CN102093159A (en) * | 2010-12-29 | 2011-06-15 | 天津市康科德科技有限公司 | Method for preparing chromatographic pure dichloromethane |
-
2011
- 2011-12-26 CN CN2011104409517A patent/CN102417434A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3631116A (en) * | 1968-01-12 | 1971-12-28 | Lothar Hornig | Process for the manufacture of carbon tetrachloride |
| CN1327952A (en) * | 2001-06-02 | 2001-12-26 | 吉林大学 | Equipment for purifying extractant of mineral oil in water and process for treating adsorbent |
| CN102093160A (en) * | 2010-12-29 | 2011-06-15 | 天津市康科德科技有限公司 | Method for preparing chromatographically-pure trichloromethane |
| CN102093159A (en) * | 2010-12-29 | 2011-06-15 | 天津市康科德科技有限公司 | Method for preparing chromatographic pure dichloromethane |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105859510A (en) * | 2016-05-09 | 2016-08-17 | 江苏梅兰化工有限公司 | Continuous production process and device of high-purity carbon tetrachloride |
| CN106040206A (en) * | 2016-07-28 | 2016-10-26 | 王金明 | Preparation method of carbon tetrachloride purification adsorbent |
| CN106238009A (en) * | 2016-07-28 | 2016-12-21 | 王金明 | A kind of preparation method of carbon tetrachloride adsorbent |
| CN107353178A (en) * | 2017-06-26 | 2017-11-17 | 江苏南大光电材料股份有限公司 | The preparation method of ultra-pure carbon tetrachloride |
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Application publication date: 20120418 |