CN107970892B - Refining agent and preparation method and application thereof - Google Patents
Refining agent and preparation method and application thereof Download PDFInfo
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- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B01J20/28057—Surface area, e.g. B.E.T specific surface area
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Abstract
The invention relates to a refining agent and a preparation method and application thereof, wherein the refining agent is activated alumina obtained by sequentially carrying out alkali treatment and acid treatment, and can be used for improving the ultraviolet transmittance of ethylene glycol products in the process of preparing ethylene glycol from synthesis gas. Compared with the prior art, the refining agent prepared by the invention does not need to load noble metal, and can greatly improve the ultraviolet transmittance of products from the ethylene glycol rectifying tower at 220nm and 275 nm.
Description
Technical Field
The invention relates to an auxiliary agent for producing ethylene glycol, in particular to a refining agent, a preparation method and application thereof, which can improve the quality of ethylene glycol products, and mainly improve the ultraviolet transmittance of ethylene glycol products produced by synthetic gas through an oxalate route.
Background
Ethylene glycol is a bulk chemical, and millions of tons of ethylene glycol are imported each year in China. 1200 ten thousand tons of glycol are consumed in 2015 in China, about 400 ten thousand tons of glycol are produced in China by oneself, and 800 ten thousand tons of glycol are imported abroad. Wherein the domestic production is divided into a petroleum route and a coal-based synthesis gas route, and the petroleum route method is to prepare the ethylene glycol from petroleum ethylene through an ethylene oxide route and is a main technical route for producing the ethylene glycol globally at present; the coal-based synthesis gas route is to use CO and H2And oxygen as raw materials, and preparing the ethylene glycol by an oxalate route. Production of ethylene glycol by petroleum method in ChinaCan not meet the market demand far away, therefore need a large amount of imports each year, on the other hand the basic national situation of our country rich coal has promoted the technological development of coal-based route production second pure. In the present year, with the successive start of 30 ten thousand tons/year ethylene glycol devices and 10 ten thousand tons/year ethylene glycol devices in new Hangzhou energy of Erdos, Anhui and the success of the start of ethylene glycol devices in multiple coal-based routes in China, the three-foot tripod standing of the three major sources of ethylene glycol, namely the petroleum route method in China, the coal-based synthesis gas method and the imported ethylene glycol in China is shown.
The coal-based synthesis gas route is another new technology for producing large chemicals which is newly developed in recent years, so the product quality, particularly the ultraviolet transmittance of ethylene glycol, is still not mature enough, and the reason is that a lot of side reactions exist in the hydrogenation process of oxalate, so that not only ethylene glycol is generated, but also other byproducts and impurities such as ethylene glycol, propylene glycol, butanediol, dimethyl ether, aldehydes, ketones and the like are generated. Through sampling analysis of a certain device, the oxalate hydrogenation product liquid contains a plurality of components such as methyl acetate, ethylene glycol monomethyl ether, methyl glycolate, ethylene glycol, methanol, 1, 2-propylene glycol, 1, 2-butanediol, 2-methoxy-1, 3-dioxolane, 2, 3-butanediol, 1-formylacetic acid, methoxyacetaldehyde, n-butanol, 2-methoxytetrahydrofuran, 2-pentanone, methoxyacetic acid ethyl ester, 3-methyl-4-hydroxy-2-butanone and the like, and some of the components can seriously affect the quality, especially the purity and the ultraviolet transmittance of the ethylene glycol product.
Chinese patent N104045516A discloses a method for improving the quality of glycol products, which mainly solves the technical problem of low ultraviolet transmittance of glycol products in the prior art. The catalyst adopts alumina as a carrier, at least one of nickel or palladium as an active component and at least one of magnesium, calcium, barium, molybdenum and cerium as an auxiliary agent. The patent needs to further load noble metal and other metals on the alumina carrier, thereby increasing the cost.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a refining agent for greatly improving the ultraviolet transmittance of a product from an ethylene glycol rectifying tower, and a preparation method and application thereof.
The purpose of the invention can be realized by the following technical scheme:
a refining agent, which is activated alumina with a specific surface area of 50-150cm obtained by alkali treatment and acid treatment in sequence2Per g, pore volume of 0.6-0.75cm3The pore diameter is 10-20 nm.
The preparation method of the refining agent comprises the steps of taking activated alumina as a raw material, firstly carrying out alkali treatment on the activated alumina, then carrying out acid treatment, washing and drying to obtain the refining agent.
Preferably, the alkali treatment is to soak the activated alumina in an alkali solution with the concentration of 1-30 wt% for 20-240 min.
More preferably, the concentration of the alkali solution adopted in the alkali treatment is 10-20 wt%, the soaking time is 60-180 min,
preferably, the base used comprises one or more of ammonia, sodium carbonate, sodium bicarbonate, potassium carbonate or potassium bicarbonate. Preferably, the activated alumina after the alkali treatment is dried for 2-8 hours at the temperature of 80-120 ℃.
Preferably, the acid treatment is to soak the activated alumina in an acid solution with the concentration of 0.1-5 wt% for 10-120 min.
More preferably, the concentration of the acid solution used in the acid treatment is 1-3 wt%, and the soaking time is 30-60 min.
Preferably, the acid used comprises one or a mixture of carbonic acid, acetic acid, oxalic acid and sulfurous acid.
Washing the activated alumina subjected to acid treatment with deionized water until the pH value of the deionized water is 6-8, and drying for 2-8 h at 80-120 ℃.
The alumina treated by acid and alkali can dredge alumina pore channels to form a space which is easy to contain trace impurities in glycol, and can promote the formation of chemical groups on the surface of the alumina, namely, various groups such as carboxyl, hydroxyl and the like and some alkaline groups are formed on the surface, and the groups have better adsorption effect on the impurities.
The prepared refining agent can be applied to the preparation of ethylene glycol from synthesis gas to improve the ultraviolet transmittance of ethylene glycol products, the obtained refining agent is sieved to 20-40 meshes, added into the ethylene glycol products according to the mass ratio of 1-3%, treated at 80-150 ℃ for 20-60 min and separated.
Compared with the prior art, the ultraviolet transmittance of the product from the ethylene glycol rectifying tower at 220nm and 275nm can be greatly improved.
Detailed Description
The method takes activated alumina as an object, firstly carries out alkali treatment, the alkali comprises at least one or a mixture of more of ammonia water, sodium carbonate, sodium bicarbonate, potassium carbonate and potassium bicarbonate, the mass concentration of the alkali in water is 1-30 wt%, the treatment time is 20-240 min, and after the alkali treatment is finished, the drying is carried out for 2-8 h at the temperature of 80-120 ℃. And after the alkali treatment is finished, drying and then carrying out acid treatment, wherein the acid comprises at least one or a mixture of more of carbonic acid, acetic acid, oxalic acid and sulfurous acid, the mass concentration of the acid in water is 0.1-5 wt%, and the treatment time is 10-120 min. And after the acid treatment is finished, washing the aluminum oxide by using deionized water until the pH value of the deionized water is 6-8, and drying the treated aluminum oxide at the temperature of 80-120 ℃ for 2-8 h.
The refining agent prepared by the method is prepared by adding a 20-40-mesh sample into an ethylene glycol product according to the mass ratio of 1-3%, treating at 80-150 ℃ for 20-60 min, and then performing rectification separation to obtain the ethylene glycol product with high ultraviolet transmittance.
The present invention will be described in detail with reference to specific examples.
Example 1
Taking activated alumina as an object, firstly, carrying out alkali treatment, wherein the alkali is ammonia water, the mass concentration is 12 wt%, the treatment time is 100min, and after the alkali treatment, drying for 8h at 80 ℃. And after the alkali treatment is finished, drying and then carrying out acid treatment, wherein the acid is oxalic acid, the mass concentration is 0.5 wt%, and the treatment time is 10 min. And after the acid treatment is finished, washing the aluminum oxide by deionized water till the pH value of the deionized water is 6.5, and drying the treated aluminum oxide at 120 ℃ for 8 hours.
The refining agent prepared by the method selects a sample of 20-40 meshes and adds the sample into an ethylene glycol product according to the mass ratio of 3%, the ethylene glycol product is treated at 80 ℃ for 60min and then is subjected to rectification separation, the ultraviolet transmittance of the ethylene glycol at 220nm is improved from 71% to 90%, and the ultraviolet transmittance at 275nm is improved from 90% to 96%.
Example 2
Taking activated alumina as an object, firstly, carrying out alkali treatment, wherein the alkali is potassium bicarbonate, the mass concentration is 20wt%, the treatment time is 180min, and after the alkali treatment, drying for 5h at 100 ℃. And after the alkali treatment is finished, drying and then carrying out acid treatment, wherein the acid is carbonic acid, the mass concentration is 3wt%, and the treatment time is 60 min. And after the acid treatment is finished, washing the aluminum oxide by deionized water till the pH value of the deionized water is 7.5, and drying the treated aluminum oxide at 100 ℃ for 6 hours.
The refining agent prepared by the method selects a sample of 20-40 meshes according to the mass ratio of 2% to be added into an ethylene glycol product, and is rectified and separated after being treated at 80 ℃ for 30min, wherein the ultraviolet transmittance of the ethylene glycol at 220nm is improved from 55% to 81%, and the ultraviolet transmittance at 275nm is improved from 84% to 94%.
Example 3
Taking activated alumina as an object, firstly, carrying out alkali treatment, wherein the alkali is sodium carbonate, the mass concentration is 28 wt%, the treatment time is 220min, and after the alkali treatment, drying at 120 ℃ for 2 h. And (3) after the alkali treatment is finished and the drying is carried out, acid treatment is carried out, the acid is sulfurous acid, the mass concentration is 2 wt%, and the treatment time is 100 min. And after the acid treatment is finished, washing the aluminum oxide by deionized water till the pH value of the deionized water is 7.8, and drying the treated aluminum oxide at 100 ℃ for 4 hours.
The refining agent prepared by the method selects a sample of 20-40 meshes according to the mass ratio of 2% to be added into an ethylene glycol product, and is rectified and separated after being treated at 100 ℃ for 60min, wherein the ultraviolet transmittance of the ethylene glycol at 220nm is improved from 67% to 89%, and the ultraviolet transmittance at 275nm is improved from 88% to 95%.
Example 4
Taking activated alumina as an object, firstly, carrying out alkali treatment, wherein the alkali is a mixture of sodium bicarbonate and ammonia water, the mass concentration of the alkali is 12 wt% of the sodium bicarbonate, the mass concentration of the ammonia water is 25%, the treatment time is 60min, and after the alkali treatment, drying the activated alumina at 120 ℃ for 2 h. And after the alkali treatment is finished, drying and then carrying out acid treatment, wherein the acid is a mixture of oxalic acid and acetic acid, the mass concentration of the mixture is 0.5 wt% and 2.5 wt%, and the treatment time is 40 min. And after the acid treatment is finished, washing the aluminum oxide by deionized water till the pH value of the deionized water is 6.8, and drying the treated aluminum oxide at 100 ℃ for 6 hours.
The refining agent prepared by the method selects a sample of 20-40 meshes according to the mass ratio of 1% to be added into an ethylene glycol product, the ethylene glycol product is rectified and separated after being treated at 120 ℃ for 45min, the ultraviolet transmittance of the ethylene glycol at 220nm is improved from 74% to 91%, and the ultraviolet transmittance at 275nm is improved from 92% to 96%.
Example 5
A refining agent is prepared from activated alumina as raw material by alkali treating, acid treating, washing, and oven drying, and has specific surface area of 50cm2Per g, pore volume of 0.6cm3(ii)/g, pore diameter is 10 nm.
In the preparation method, the alkali treatment is to put the activated alumina into ammonia water solution with the concentration of 1 wt% for soaking for 240min, and the activated alumina after the alkali treatment is dried for 8h at the temperature of 80 ℃.
The acid treatment is to soak the activated alumina in 0.1 wt% carbonic acid solution for 120 min. The activated alumina after acid treatment is washed by deionized water until the pH value of the deionized water is 6, and then dried for 8 hours at 80 ℃.
The alumina treated by acid and alkali can dredge alumina pore channels to form a space which is easy to contain trace impurities in glycol, and can promote the formation of chemical groups on the surface of the alumina, namely, various groups such as carboxyl, hydroxyl and the like and some alkaline groups are formed on the surface, and the groups have better adsorption effect on the impurities. The ultraviolet transmittance of the product from the ethylene glycol rectifying tower at 220nm and 275nm can be greatly improved. The prepared refining agent is applied to the preparation of ethylene glycol from synthesis gas to improve the ultraviolet transmittance of an ethylene glycol product, the obtained refining agent is sieved to 20 meshes, added into the ethylene glycol product according to the mass ratio of 1%, treated at 80 ℃ for 60min and separated.
Example 6
A refining agent is prepared from activated alumina as raw material by alkali treating, acid treating, washing, and oven drying, and has specific surface area of 80cm2Per g, pore volume of 0.7cm3G, pore diameter of 20 nm.
In the preparation method, the alkali treatment is to put the activated alumina into a sodium carbonate solution with the concentration of 10 wt% for soaking for 180min, and the activated alumina after the alkali treatment is dried for 4h at the temperature of 100 ℃.
The acid treatment is to soak the activated alumina in 1 wt% acetic acid solution for 60min, wash the activated alumina after the acid treatment with deionized water until the pH value of the deionized water is 7, and then dry the activated alumina at 100 ℃ for 6 h.
The alumina treated by acid and alkali can dredge alumina pore channels to form a space which is easy to contain trace impurities in glycol, and can promote the formation of chemical groups on the surface of the alumina, namely, various groups such as carboxyl, hydroxyl and the like and some alkaline groups are formed on the surface, and the groups have better adsorption effect on the impurities. The ultraviolet transmittance of the product from the ethylene glycol rectifying tower at 220nm and 275nm can be greatly improved. The prepared refining agent is applied to the preparation of ethylene glycol from synthesis gas to improve the ultraviolet transmittance of an ethylene glycol product, the obtained refining agent is sieved to 30 meshes, added into the ethylene glycol product according to the mass ratio of 2%, treated at 100 ℃ for 40min and separated.
Example 7
A refining agent is prepared from activated alumina as raw material by alkali treating, acid treating, washing, and oven drying, and has specific surface area of 100cm2Per g, pore volume of 0.7cm3G, pore diameter of 15 nm.
In the preparation method, the alkali treatment is to soak the activated alumina in a sodium bicarbonate solution with the concentration of 20wt% for 60min, and the activated alumina after the alkali treatment is dried for 4h at the temperature of 100 ℃.
The acid treatment is to soak the activated alumina in 1 wt% sulfurous acid solution for 30min, wash the activated alumina after the acid treatment with deionized water until the pH value of the deionized water is 7, and then dry the activated alumina at 100 ℃ for 6 h.
The alumina treated by acid and alkali can dredge alumina pore channels to form a space which is easy to contain trace impurities in glycol, and can promote the formation of chemical groups on the surface of the alumina, namely, various groups such as carboxyl, hydroxyl and the like and some alkaline groups are formed on the surface, and the groups have better adsorption effect on the impurities. The ultraviolet transmittance of the product from the ethylene glycol rectifying tower at 220nm and 275nm can be greatly improved. The prepared refining agent is applied to the preparation of ethylene glycol from synthesis gas to improve the ultraviolet transmittance of an ethylene glycol product, the obtained refining agent is sieved to 30 meshes, added into the ethylene glycol product according to the mass ratio of 2%, treated at 100 ℃ for 40min and separated.
Example 8
A refining agent is prepared from activated alumina as raw material by alkali treating, acid treating, washing, and oven drying, and has specific surface area of 150cm2Per g, pore volume of 0.75cm3G, pore diameter of 18 nm.
In the preparation method, the alkali treatment is to soak the activated alumina in a potassium carbonate solution with the concentration of 30 wt% for 20min, and the activated alumina after the alkali treatment is dried for 2h at 120 ℃.
The acid treatment is to put the activated alumina into oxalic acid solution with the concentration of 5 wt% to be soaked for 10min, the activated alumina after the acid treatment is washed by deionized water until the pH value of the deionized water is 8, and then the activated alumina is dried for 2h at the temperature of 120 ℃.
The alumina treated by acid and alkali can dredge alumina pore channels to form a space which is easy to contain trace impurities in glycol, and can promote the formation of chemical groups on the surface of the alumina, namely, various groups such as carboxyl, hydroxyl and the like and some alkaline groups are formed on the surface, and the groups have better adsorption effect on the impurities. The ultraviolet transmittance of the product from the ethylene glycol rectifying tower at 220nm and 275nm can be greatly improved. The prepared refining agent is applied to the preparation of ethylene glycol from synthesis gas to improve the ultraviolet transmittance of an ethylene glycol product, the obtained refining agent is sieved to 40 meshes, added into the ethylene glycol product according to the mass ratio of 3 percent, treated at 150 ℃ for 20min and separated.
Claims (4)
1. The preparation method of the refining agent is characterized by comprising the following steps:
taking activated alumina as a raw material, firstly, carrying out alkaline soaking treatment on the activated alumina, wherein during the alkaline soaking treatment, the concentration of adopted alkaline liquor is 10-20 wt%, and the soaking time is 60-180 min;
drying the activated alumina subjected to alkali treatment for 2-8 h at 80-120 ℃;
then washing after acid soaking treatment, wherein the concentration of an acid solution adopted in the acid treatment is 1-3 wt%, and the soaking time is 30-60 min;
washing the activated alumina subjected to acid treatment with deionized water until the pH value of the deionized water is 6-8, and drying at 80-120 ℃ for 2-8 h to obtain a refining agent with the specific surface area of 50-150 m2A pore volume of 0.6-0.75 cm/g3The pore diameter is 10-20 nm.
2. The method for preparing a refining agent according to claim 1, wherein the alkali used comprises one or a mixture of ammonia, sodium carbonate, sodium bicarbonate, potassium carbonate or potassium bicarbonate.
3. The method for preparing a refining agent according to claim 1, wherein the acid used comprises one or a mixture of carbonic acid, acetic acid, oxalic acid, sulfurous acid.
4. The application of the refining agent obtained by the preparation method of claim 1, wherein the refining agent is applied to the preparation of ethylene glycol from synthesis gas to improve the ultraviolet transmittance of an ethylene glycol product, the obtained refining agent is sieved to 20-40 meshes, added into the ethylene glycol product according to the mass ratio of 1-3%, treated at 80-150 ℃ for 20-60 min and separated.
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| CN112439412B (en) * | 2019-09-02 | 2023-06-06 | 中国石油化工股份有限公司 | Refining agent for ethylene glycol hydrofining and preparation method thereof |
| CN111644172B (en) * | 2019-09-09 | 2023-12-01 | 上海浦景化工技术股份有限公司 | Catalyst for liquid phase hydrogenation and preparation method and application thereof |
| CN113620780A (en) * | 2021-08-06 | 2021-11-09 | 联泓新材料科技股份有限公司 | Method for intermittently preparing polyester-grade ethylene glycol from industrial-grade ethylene glycol |
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