CN101544551A - Method for purifying high-purity organic solvent-acetone for scientific research - Google Patents

Abstract

The invention relates to a method for purifying a high-purity organic solvent-acetone for scientific research, which comprises the following steps that: acetone as the raw material is adsorbed to remove impurities by an adsorption resin, dried to remove water by a drying agent, rectified by a rectifying still, filtered and packaged to obtain a chromatographic grade and pesticide residue grade acetone product. The method can obtain the chromatographic acetone product with the purity more than 99.9 percent, ensure that the yield is more than 93 percent and the qualification rate is more than 95 percent, can obtain a 50 to 60 percent pesticide residue grade acetone reagent, can meet the application demand of high efficiency liquid chromatography (HPLC) customers on pesticide residue, and fill in the gap of the national production of pesticide residue grade chromatography reagents; and at the same time, compared with the prior method, the method has high product purity, simple and convenient operation and stable operation, and is suitable for mass production.

Description

A kind of purification method of high-purity organic solvent acetone for scientific research

technical field

The invention belongs to the technical field of chemical industry and relates to a method for purifying an organic solvent, in particular to a method for purifying acetone, a high-purity organic solvent used in scientific research.

Background technique

The acetone reagent sold on the market has an acetone content of about 99.5%, which contains a small amount of unsaturated hydrocarbons, water and other impurities. This kind of acetone cannot meet the needs of relevant scientific research experiments, so this kind of acetone must be further purified so that its various technical indicators can reach the standards of chromatographic grade and pesticide residue grade acetone before it can be used.

At present, domestic information on acetone purification mostly focuses on the recovery and utilization of acetone in waste liquid. The patent numbers are: 200710028462.4 and 200710060107.5 respectively provide related methods and devices for the recovery of acetone in waste liquid, but they are not applicable In the purification of high-purity acetone (content 99.5%).

According to the search, there are very few related elaborations on further purification methods of high-purity acetone reagents in China, mainly because the content of impurities in acetone through preliminary purification is small, and it is difficult to remove impurities in rectification. Therefore, the present invention is aimed at this technology. Problems come up with effective solutions.

Contents of the invention

The object of the present invention is to provide a method for purifying acetone, a high-purity organic solvent for scientific research, which has the characteristics of simple process, easy separation of residues, and high product purity.

The present invention is implemented through the following scheme:

A kind of purification method of high-purity organic solvent acetone for scientific research, the step of purification is as follows:

(1) the raw material acetone is passed through the adsorption resin column to remove impurities;

(2) dry the acetone after adsorption, and measure the water content;

(3) Carry out rectification to the acetone with moisture content in the acceptable range after drying, and filter after rectification to obtain chromatographic grade and pesticide residue grade acetone products.

Moreover, the adsorption resin is Amberlite XAD-4, and the desiccant is anhydrous potassium sulfate or anhydrous potassium carbonate.

Moreover, the raw material acetone flows through the adsorption resin column at a speed of 20-80mL/min.

Moreover, the qualified water content range in the acetone in the step (3) is controlled at ≤0.2%.

Moreover, the conditions for rectifying the dried acetone are as follows: the temperature at the bottom of the rectification tank is 100-300°C, the temperature of the acetone liquid in the tank is 61-65°C, the temperature at the top of the tank is 55-57°C, and the reflux ratio is controlled at 1 : 3~5.

Advantage and positive effect of the present invention are:

1. The present invention uses acetone with a content of 99.5% as a raw material, uses an adsorption resin as an adsorbent to carry out adsorption and separation to remove impurities therein, uses anhydrous potassium sulfate or anhydrous potassium carbonate as a desiccant to remove moisture therein, and undergoes adsorption and drying. 1. The acetone product with a purity of 99.9% is obtained by rectification and purification. The purification method is simple, the residue is easy to separate, the product has high purity, stable operation, and is suitable for large-scale production.

2. This purification method uses adsorption resin to absorb and remove impurities in acetone, and the content of acetone is increased to 99.9%. It reduces energy consumption, is more suitable for industrial production and application, and has significant economic benefits.

3, the product produced by this purification method meets the requirements of chromatographic grade and pesticide residue grade chromatographic acetone after testing its various indicators, its acetone content is greater than 99.9%, the recovery rate is greater than 93%, and the yield of finished product reaches 95%, wherein 50- 60% pesticide residue-grade acetone reagent, this product can meet the application needs of high-performance liquid chromatography (HPLC) customers in pesticide residues, and fills the gap in the domestic production of pesticide residue-grade reagents.

specific embodiment

The present invention will be further described in detail below through the specific examples, the following examples are only descriptive, not restrictive, and cannot limit the protection scope of the present invention with this.

Example 1:

A kind of purification method of high-purity organic solvent acetone for scientific research, the steps are as follows:

(1) Lift the raw acetone (content is about 99.5%) above the adsorption tower, wherein the adsorption tower is 2M high, 10cm in diameter, and the amount of adsorption resin inside is 4/5 of the tower height, and the acetone raw material is adsorbed at a speed of 20mL/min ; In the tower, acetone is fully contacted with the adsorption resin, so that the unsaturated hydrocarbon impurities are adsorbed, and the quality of the adsorbed liquid is detected, and the quality of the adsorbed liquid is tested to be qualified (that is, the indicators of the effluent are close to the chromatographic level and the technology of the pesticide residue level. Index requirements, its specific technical index requirements are shown in Table 1), enter the next step operation, and remove the fraction before adsorption with high impurity.

(2) The acetone flowing out of the above-mentioned adsorption tower enters the drying tower, the tower height is 2M, and the diameter is 10cm, and the anhydrous potassium sulfate through baking and drying is loaded into, and the water content of the acetone after measurement is dried, and the moisture is controlled at ≤0.2%. Enter the next step after passing the test; if the moisture content is greater than 0.25%, it means that the desiccant has been saturated with water and must be replaced before drying.

(3) Pour the above-mentioned dried acetone into a 100L stainless steel rectification kettle for rectification, use heat conduction oil to heat, control the bottom temperature of the stainless steel kettle to 100°C, the temperature of the acetone liquid in the kettle to 61°C, the temperature of the liquid out to 55°C, and control the reflux The liquid is discharged at a ratio of 1:3, and the finished product is filtered through a 0.45 μm NYL microporous membrane, bottled and sealed under nitrogen protection, and a qualified chromatographic grade and pesticide residue grade acetone product (purity 99.9%) is obtained. deal with.

Example 2:

A kind of purification method of high-purity organic solvent acetone for scientific research, the steps are as follows:

(1) The raw material acetone (content is about 99.5%) is lifted above the adsorption tower, the adsorption tower is 2M high, the diameter is 10cm, the amount of built-in adsorption resin is 4/5 of the tower height, and the acetone raw material is adsorbed at a speed of 80mL/min, After the adsorption effluent is qualified, enter the next step of operation; and remove the fraction with high impurities before adsorption.

(2) The effluent of the above-mentioned adsorption tower is entered into the drying tower, the tower height is 2M, and the diameter is 10cm, and the anhydrous potassium carbonate through baking and drying is packed into, and the moisture content of the acetone after measurement is dried, and the moisture content is controlled at ≤0.2%. Enter the next step after passing the test; when the moisture content is greater than 0.25%, it means that the desiccant has been saturated with water and must be replaced before drying.

(3) The above-mentioned dried acetone is injected into a 120L stainless steel distillation still for rectification. Use heat conduction oil to heat, control the temperature at the bottom of the stainless steel kettle to 300°C, the temperature of the acetone liquid in the kettle to 65°C, and the liquid outlet temperature to 57°C, and control the reflux ratio to 1:5. Bottling under protection is sealed to obtain qualified chromatographic grade and pesticide residue grade acetone products (purity 99.9%); the preceding fraction is further processed.

Determination of pesticide residue level indicators:

Pesticide level indicators: In addition to meeting the chromatographic level indicators, after the sample is concentrated 300 times, all the miscellaneous peaks detected by GC-ECD gas chromatography (compared with the peak height of γ-HCH) are all lower than 10ng/L, and the pesticide Residual grade is qualified. The purified high-purity acetone can be further purified to obtain 50-60% pesticide residue grade chromatographic acetone product.

Table 1: Technical indicators of raw materials, chromatography, and pesticide residue grade acetone

Claims (5)

1, a kind of method of purification of high-purity organic solvent-acetone for scientific research is characterized in that: the step of purification is as follows:

(1) with raw material acetone by adsorption resin column to remove impurity;

(2) acetone after will adsorbing carries out drying, and measures water content;

(3) water content after the drying is carried out rectifying at the acetone of acceptability limit, the rectifying after-filtration promptly obtains chromatographic grade and pesticide-residue-level acetone product.

2, the method for purification of a kind of high-purity organic solvent-acetone for scientific research according to claim 1 is characterized in that: described polymeric adsorbent is Amberlite XAD-4, and siccative is anhydrous potassium sulfate or Anhydrous potassium carbonate.

3, the method for purification of a kind of high-purity organic solvent-acetone for scientific research according to claim 1 is characterized in that: described raw material acetone with the 20-80mL/min velocity flow through adsorption resin column.

4, the method for purification of a kind of high-purity organic solvent-acetone for scientific research according to claim 1 is characterized in that: in the described step (3) in the acetone qualified water content ranges be controlled at≤0.2%.

5, the method for purification of a kind of high-purity organic solvent-acetone for scientific research according to claim 1, it is characterized in that: the described condition that dried acetone is carried out rectifying is: temperature is 100～300 ℃ at the bottom of the rectifying still, the acetone fluid temperature is 61 ℃～65 ℃ in the still, 55 ℃～57 ℃ of still top temperature, control reflux ratio 1:3～5.