CN110642707B - Purification production method of low-cost environment-friendly sodium salicylate - Google Patents
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Abstract
The invention discloses a low-cost purification production method of environment-friendly sodium salicylate, which comprises the following steps: step 1, putting a sodium salicylate raw material into a closed container, adding pure water, stirring and soaking, dehydrating after completely soaking, and then dissolving by using the pure water; step 2, after complete dissolution, adding ethylene diamine tetraacetic acid into the solution, continuously stirring, and then carrying out heat preservation and precipitation; step 3, after heat preservation and precipitation, filtering the solution, and then concentrating, cooling and crystallizing; and 4, after the crystallization is completed, performing dehydration treatment to obtain primary crystals, and performing crystal drying treatment on the primary crystals to finally obtain the product. According to the invention, the primary purification effect is improved and the recrystallization times are reduced by adopting chelate impurity removal and aqueous solution impurity removal modes, so that the production cost of an enterprise is greatly reduced, the profit margin of the enterprise is improved and the defects of the existing production method are overcome under the condition that the product meets the environmental protection level requirement.
Description
Technical Field
The invention relates to the technical field of sodium salicylate purification, in particular to a low-cost environment-friendly sodium salicylate purification production method.
Background
Sodium salicylate is a white flake or powder, soluble in water, glycerol, insoluble in ether, chloroform, benzene, mainly used in analgesics and rheumatics, and also used as an organic synthesis and analysis reagent, and is generally prepared by: adding salicylic acid and sodium bicarbonate into distilled water alternately, keeping the temperature at 60 deg.C, keeping the solution in an acidic state, and adding appropriate amount of ethylenediaminetetraacetic acid (EDTA) and sodium hydrosulfite. The temperature is increased to 85 ℃ and the reaction is carried out for half an hour. Filtering the qualified reaction liquid, sending the reaction liquid into a boiling bed, and drying the reaction liquid at 85 ℃ to obtain the sodium salicylate.
At present, the high-purity environment-friendly sodium salicylate has wide application in the aspects of biological medicine, chemical analysis and the like, and the main product indexes of the high-purity environment-friendly sodium salicylate are as follows: purity is not less than 99.5 wt%, water insoluble matter is not more than 0.005 wt%, and ammonia content is not more than 0.001 wt%. Generally, the sodium salicylate prepared by synthesis belongs to industrial grade products, contains more impurities, such as heavy metal, salicylic acid and the like, can not be directly used as environment-friendly grade sodium salicylate, and can be used only after the sodium salicylate is purified to meet the high purity requirement, at present, the main industrial purification method for the sodium salicylate comprises the following steps: after sodium salicylate is dissolved by pure water, insoluble impurities are filtered, then the sodium salicylate is concentrated, cooled, crystallized and dehydrated to obtain primary crystals, the primary crystals are repeatedly dissolved, concentrated, cooled, crystallized and dehydrated, the sodium salicylate is purified for a plurality of times in a recrystallization mode for 3-5 times, and finally the requirement of a high-purity environment-friendly product (namely an aqueous solution recrystallization purification refining process) is met.
Chinese patent CN107098809A discloses a purification and refining method of high-purity sodium salicylate, which comprises the following steps: under the condition of water bath heating, mixing and stirring the sodium salicylate raw material, ethanol and activated carbon together, then filtering for multiple times, heating, concentrating and crystallizing, recycling mother liquor, and drying crystals to obtain the sodium salicylate. This method replaces pure water with ethanol, and adsorbs precipitated particles with activated carbon, and although ethanol can be recovered and utilized, there are several disadvantages: 1. the ethanol has large usage amount and energy consumption, 50kg of sodium salicylate raw material is generally used as a batch for industrial production, 270L of 95 wt% ethanol is needed for each batch, the usage amount is large, the energy consumption for later-stage water bath and distillation recovery is large, the ethanol has strong volatility, the ethanol loss in the production process is large, and the production cost is obviously higher than that of a recrystallization refining mode of aqueous solution; 2. the impurity content of the mother liquor is high, the purity is influenced by recycling, when the ethanol is used as a solvent, some organic impurities and heavy metals are dissolved in the mother liquor, the impurities are trace and cannot be removed through activated carbon adsorption, after the mother liquor is recycled, the content of the impurities is too small, and the impurities are wrapped in the crystals during later-stage heating, concentration and crystallization, so that the content of the crystallized impurities is increased, and the purity of the final product can not reach the standard. Therefore, the purification mode can not be used for solving the problem of producing high-purity environment-friendly sodium salicylate with low cost by enterprises.
Disclosure of Invention
The invention aims to: aiming at the existing problems, the purification production method of the low-cost environment-friendly sodium salicylate is provided, a small amount of Ethylene Diamine Tetraacetic Acid (EDTA) is added after the sodium salicylate raw material is dissolved, and the obtained product meets the environment-friendly requirement under the condition of reducing the recrystallization times through chelate impurity removal and aqueous solution impurity removal double impurity removal treatment, so that the production cost is greatly reduced, the enterprise profit space is improved, and the defects of the existing production method are overcome.
The technical scheme adopted by the invention is as follows: the purification production method of the low-cost environment-friendly sodium salicylate is characterized by comprising the following steps:
step 1, putting a sodium salicylate raw material into a closed container, adding pure water, stirring and soaking, dewatering after complete soaking, dissolving the soaked sodium salicylate raw material with the pure water, controlling the dissolving temperature to be below 60 ℃, and stirring to fully dissolve the sodium salicylate raw material;
step 2, after complete dissolution, adding ethylene diamine tetraacetic acid into the solution, continuously stirring, and then carrying out heat preservation and precipitation;
step 3, after heat preservation and precipitation, filtering the solution, and then concentrating, cooling and crystallizing;
and 4, after the crystallization is completed, performing dehydration treatment to obtain primary crystals, and performing crystal drying treatment on the primary crystals to finally obtain the product.
In the method, the raw material is soaked for pre-impurity removal treatment of the raw material to remove most impurities in the raw material, good purification conditions are provided for a later-stage deep purification process, if the raw material is directly and completely dissolved by pure water, the solution contains more impurities, the consumption of the solution is very large no matter impurity substances are added or the pure water is directly used for filtering and removing impurities, ideal purification effect can be achieved through repeated continuous purification, the production cost is high, therefore, the production cost of an enterprise can be obviously reduced by soaking the raw material, most impurities on the surface of the raw material can be removed, and the influence of the impurities on the subsequent purification process is avoided. Furthermore, the method of the invention is mainly characterized in that after the raw materials are fully dissolved, ethylenediamine tetraacetic acid (EDTA) is added into the solution, the EDTA is a commonly used chelating agent, for example, the EDTA can be used in the synthesis of sodium salicylate, but in the purification process of sodium salicylate, no application precedent exists, the EDTA is added into the sodium salicylate solution, mainly in order to remove metal ions and heavy metal ions in the solution, organic matters such as salicylic acid in the sodium salicylate solution are removed by pure water, the formed chelate is flocculated with suspended matters and other insoluble impurities in the solution, thereby accelerating the precipitation speed, when the solution is subjected to heat preservation and precipitation, the impurities in the solution are removed completely, so that the primary precipitation effect is optimal, and when the subsequent cooling crystallization and dehydration treatment are carried away by pure water through dilution and filtration, the remaining soluble impurities and organic matters are removed, the obtained primary crystallization has extremely low impurity content, if the raw material has high purity (for example, the raw material is of analytical pure grade), two purification effects can be achieved only by one-time crystallization, and then an environment-friendly product can be obtained only by crystal drying treatment, compared with the traditional purification process of aqueous solution recrystallization only using pure water, the traditional process can achieve the environment-friendly requirement by 3-5 times of recrystallization purification even on the raw material with high purity, although the invention introduces the ethylenediaminetetraacetic acid, the addition amount is extremely low (the addition ratio is generally 1:100), most of the raw material is filtered out by forming chelate, the residual extremely low content is discharged by subsequent filtering and concentration processes, therefore, the purity of the formed crystal is almost not influenced, and the purification times only need 1-time crystallization, even for industrial-grade raw materials with lower purity, the purification frequency is only required to be carried out for 2 times, obviously, the production cost and the production period are obviously reduced, the technical effect has obvious advantages, and the traditional process cannot achieve the effect, so the invention solves the problem that the enterprises cannot produce high-purity environment-friendly sodium salicylate at low cost at present by adopting a chelate impurity removal mode and an aqueous solution impurity removal mode.
In the present invention, the purpose of soaking is to pre-remove impurities, so in order to better exert the effect and reduce the negative effect of soaking, the mass ratio of the pure water used for soaking to the sodium salicylate raw material is preferably within the range of (1-2):5, if the mass ratio is beyond the range, the soaking effect is deteriorated, namely if the pure water is too much, the raw material is more lost, if the pure water is too little, the soaking effect can not be achieved, after the inventor tests, the mass ratio of the pure water to the sodium salicylate raw material is preferably within the range of (1-2):5, such as 1:5, 2:5, 1.4:5, 1.5:5 and 1.6:5, and further such as 1.2:5 and 1.3:5, and the specific ratio can be selected according to the actual use.
Further, in order to ensure sufficient soaking, the inventor tests for many times to obtain the method, and the soaking time needs to be more than 20 hours to ensure sufficient soaking. Of course, the soaking time is related to the amount of raw materials, the soaking time is longer when the amount is larger, and the soaking time is shorter when the amount is smaller, and the soaking time can be lower than 20h for small-scale or experimental purification, but the soaking time is not shorter than 20h for industrial production.
Furthermore, in the step 2, the usage amount of the ethylenediaminetetraacetic acid needs to be in a proper range to fully exert the effect, the inventor tests for a plurality of times to obtain the ethylenediaminetetraacetic acid solution, the mass ratio of the addition amount of the ethylenediaminetetraacetic acid to the solution is (1-3):200 is proper, if the addition amount of the ethylenediaminetetraacetic acid is lower than the mass ratio of the solution, the impurity removal effect of the ethylenediaminetetraacetic acid is poor, a qualified product cannot be obtained only through one-time crystallization, and if the addition amount of the ethylenediaminetetraacetic acid is higher than the mass ratio of the solution, more ethylenediaminetetraacetic acid remains in the solution, and the crystallization purity is adversely affected.
Further, in the step 2, in order to ensure that sufficient precipitation is carried out, the heat preservation and precipitation time is 1-3h, and the cooling temperature is controlled below 20 ℃.
In the invention, for the condition that the purity of the raw material is not good enough, the primary crystal is completely dissolved by pure water and then is recrystallized for the second time, then the secondary crystal is obtained by dehydration, and the product is finally obtained after the secondary crystal is subjected to crystal drying treatment. The invention mainly removes impurities and purifies by a chelating agent before primary crystallization, thereby improving the purification effect, reducing the subsequent purification times and further achieving the purpose of reducing the production cost of enterprises.
Furthermore, the crystal drying temperature of the crystal drying treatment is below 60 ℃, and the crystal drying time is more than 8 h.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that: according to the invention, the primary purification effect is improved and the recrystallization times are reduced by adopting a chelate impurity removal and aqueous solution impurity removal dual impurity removal treatment mode, so that the production cost of an enterprise is greatly reduced under the condition that the product meets the environmental protection level requirement, the profit margin of the enterprise is improved, the defects of the existing production method are overcome, and the low-cost environmental protection level sodium salicylate purification production method suitable for industrial application is provided for the enterprise.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A low-cost purification production method of environment-friendly sodium salicylate comprises the following steps:
step 1, 50kg of analytically pure sodium salicylate raw material is placed into a closed container, then 10kg of pure water is added for complete soaking, and stirring is continuously carried out, wherein the soaking time is 30 hours;
step 2, after soaking, performing dehydration treatment, performing additional treatment on a dehydrated solution, dissolving the soaked sodium salicylate raw material by using pure water, controlling the dissolving temperature to be below 60 ℃, and stirring to fully dissolve the sodium salicylate raw material;
step 3, after complete dissolution, adding 2kg of ethylenediamine tetraacetic acid into the solution, continuously stirring, and then carrying out heat preservation and precipitation for 3 hours;
step 4, after heat preservation and precipitation, filtering the solution, then concentrating, cooling and crystallizing, wherein the cooling temperature is controlled below 20 ℃;
step 5, after the crystallization is completed, carrying out dehydration treatment to obtain primary crystallization, and additionally treating the dehydrated solution;
and 6, carrying out crystal drying treatment on the primary crystal in a vacuum drying oven, wherein the crystal drying temperature is below 60 ℃, and the crystal drying time is 9 hours, thus obtaining the product finally.
Example 2
A low-cost purification production method of environment-friendly sodium salicylate comprises the following steps:
step 1, 50kg of analytically pure sodium salicylate raw material is placed into a closed container, then 20kg of pure water is added for complete soaking, and stirring is continuously carried out, wherein the soaking time is 20 hours;
step 2, after soaking, performing dehydration treatment, performing additional treatment on a dehydrated solution, dissolving the soaked sodium salicylate raw material by using pure water, controlling the dissolving temperature to be below 60 ℃, and stirring to fully dissolve the sodium salicylate raw material;
step 3, after complete dissolution, adding 1kg of ethylenediamine tetraacetic acid into the solution, continuously stirring, and then carrying out heat preservation and precipitation for 1 h;
step 4, after heat preservation and precipitation, filtering the solution, then concentrating, cooling and crystallizing, wherein the cooling temperature is controlled below 20 ℃;
step 5, after the crystallization is completed, carrying out dehydration treatment to obtain primary crystallization, and additionally treating the dehydrated solution;
and 6, carrying out crystal drying treatment on the primary crystal in a vacuum drying oven, wherein the crystal drying temperature is below 60 ℃, and the crystal drying time is 8 hours, thus finally obtaining the product.
Example 3
A low-cost purification production method of environment-friendly sodium salicylate comprises the following steps:
step 1, putting 50kg of analytically pure sodium salicylate raw material into a closed container, then adding 13kg of pure water to completely soak, and continuously stirring, wherein the soaking time is 25 hours;
step 2, after soaking, performing dehydration treatment, performing additional treatment on a dehydrated solution, dissolving the soaked sodium salicylate raw material by using pure water, controlling the dissolving temperature to be below 60 ℃, and stirring to fully dissolve the sodium salicylate raw material;
step 3, after complete dissolution, adding 2kg of ethylenediamine tetraacetic acid into the solution, continuously stirring, and then carrying out heat preservation and precipitation for 2 hours;
step 4, after heat preservation and precipitation, filtering the solution, then concentrating, cooling and crystallizing, wherein the cooling temperature is controlled below 20 ℃;
step 5, after the crystallization is completed, carrying out dehydration treatment to obtain primary crystallization, and additionally treating the dehydrated solution;
and 6, carrying out crystal drying treatment on the primary crystal in a vacuum drying oven, wherein the crystal drying temperature is below 60 ℃, and the crystal drying time is over 10 hours, thus finally obtaining the product.
Example 4
A low-cost purification production method of environment-friendly sodium salicylate comprises the following steps:
step 1, putting 50kg of industrial grade sodium salicylate raw material into a closed container, then adding 14kg of pure water to completely soak, and continuously stirring, wherein the soaking time is 25 hours;
step 2, after soaking, performing dehydration treatment, performing additional treatment on a dehydrated solution, dissolving the soaked sodium salicylate raw material by using pure water, controlling the dissolving temperature to be below 60 ℃, and stirring to fully dissolve the sodium salicylate raw material;
step 3, after complete dissolution, adding 3kg of ethylenediamine tetraacetic acid into the solution, continuously stirring, and then carrying out heat preservation and precipitation for 3 hours;
step 4, after heat preservation and precipitation, filtering the solution, then concentrating, cooling and crystallizing, wherein the cooling temperature is controlled below 20 ℃;
step 5, after the crystallization is completed, carrying out dehydration treatment to obtain primary crystallization, and additionally treating the dehydrated solution;
step 6, completely dissolving the primary crystals by using pure water, then carrying out secondary recrystallization, and then dehydrating to obtain secondary crystals;
and 7, carrying out crystal drying treatment on the secondary crystal in a vacuum drying oven, wherein the crystal drying temperature is below 60 ℃, and the crystal drying time is 11 hours, thus obtaining the product finally.
Example 5
A low-cost purification production method of environment-friendly sodium salicylate comprises the following steps:
step 1, putting 50kg of industrial grade sodium salicylate raw material into a closed container, then adding 15kg of pure water to completely soak, and continuously stirring, wherein the soaking time is 26 hours;
step 2, after soaking, performing dehydration treatment, performing additional treatment on a dehydrated solution, dissolving the soaked sodium salicylate raw material by using pure water, controlling the dissolving temperature to be below 60 ℃, and stirring to fully dissolve the sodium salicylate raw material;
step 3, after complete dissolution, adding 2kg of ethylenediamine tetraacetic acid into the solution, continuously stirring, and then carrying out heat preservation and precipitation for 3 hours;
step 4, after heat preservation and precipitation, filtering the solution, then concentrating, cooling and crystallizing, wherein the cooling temperature is controlled below 20 ℃;
step 5, after the crystallization is completed, carrying out dehydration treatment to obtain primary crystallization, and additionally treating the dehydrated solution;
step 6, completely dissolving the primary crystals by using pure water, then carrying out secondary recrystallization, and then dehydrating to obtain secondary crystals;
and 7, carrying out crystal drying treatment on the secondary crystal in a vacuum drying oven, wherein the crystal drying temperature is below 60 ℃, and the crystal drying time is 10 hours, thus obtaining the product finally.
Example 6
A low-cost purification production method of environment-friendly sodium salicylate comprises the following steps:
step 1, putting 50kg of industrial grade sodium salicylate raw material into a closed container, then adding 18kg of pure water to completely soak, and continuously stirring for 24 hours;
step 2, after soaking, performing dehydration treatment, performing additional treatment on a dehydrated solution, dissolving the soaked sodium salicylate raw material by using pure water, controlling the dissolving temperature to be below 60 ℃, and stirring to fully dissolve the sodium salicylate raw material;
step 3, after complete dissolution, adding 2kg of ethylenediamine tetraacetic acid into the solution, continuously stirring, and then carrying out heat preservation and precipitation for 1-3 h;
step 4, after heat preservation and precipitation, filtering the solution, then concentrating, cooling and crystallizing, wherein the cooling temperature is controlled below 20 ℃;
step 5, after the crystallization is completed, carrying out dehydration treatment to obtain primary crystallization, and additionally treating the dehydrated solution;
step 6, completely dissolving the primary crystals by using pure water, then carrying out secondary recrystallization, and then dehydrating to obtain secondary crystals;
and 7, carrying out crystal drying treatment on the secondary crystal in a vacuum drying oven, wherein the crystal drying temperature is below 60 ℃, and the crystal drying time is 10 hours, thus obtaining the product finally.
The test data for the products obtained in examples 1 to 6 above are shown in the following table:
TABLE 1 raw assay data for samples run Nos. 1-6 (examples 1-6)
As shown in Table 1, the products obtained in the 6 embodiments all meet the environmental protection level requirements, which shows that the low-cost environmental protection level sodium salicylate purification production method provided by the invention is successful, and the problems of overhigh production cost and low enterprise profit of the traditional method are solved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (4)
1. The purification production method of the low-cost environment-friendly sodium salicylate is characterized by comprising the following steps:
step 1, putting a sodium salicylate raw material into a closed container, adding pure water, stirring and soaking, wherein the mass ratio of the pure water for soaking to the sodium salicylate raw material is (1-2):5, the soaking time is more than 20 hours, after complete soaking, dehydrating, dissolving the soaked sodium salicylate raw material by using the pure water, controlling the dissolving temperature to be below 60 ℃, and stirring to fully dissolve the sodium salicylate raw material;
step 2, after complete dissolution, adding ethylene diamine tetraacetic acid into the solution and continuously stirring, wherein the mass ratio of the addition amount of the ethylene diamine tetraacetic acid to the solution is (1-3):200, and then carrying out heat preservation and precipitation;
step 3, after heat preservation and precipitation, filtering the solution, and then concentrating, cooling and crystallizing;
and 4, after the crystallization is completed, performing dehydration treatment to obtain primary crystals, and performing crystal drying treatment on the primary crystals to finally obtain the product.
2. The method for purifying and producing sodium salicylate of low cost and environmental protection grade as claimed in claim 1, wherein the time of heat preservation and precipitation is 1-3h in step 2, and the cooling temperature is controlled below 20 ℃ in step 3.
3. The method for purifying and producing sodium salicylate of low cost and environmental protection grade as claimed in claim 1, wherein the primary crystallization is completely dissolved by pure water and then is recrystallized for the second time, and then is dehydrated to obtain the secondary crystallization, and the secondary crystallization is dried to obtain the final product.
4. The purification production method of low-cost environmental-friendly sodium salicylate as claimed in claim 1, wherein the crystal baking temperature of the crystal baking treatment is below 60 ℃, and the crystal baking time is above 8 h.
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