A method for producing high-purity chloromethyl ether
By using a composite catalyst in the production of chloromethyl ethyl ether and utilizing iron-calcium dual active sites supported on a carbon fiber skeleton, the problems of low purity and high cost of chloromethyl ethyl ether have been solved, and the efficient production of high-purity products has been achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- PINGDINGSHAN SHENYING CHEM TECH CO LTD
- Filing Date
- 2026-02-02
- Publication Date
- 2026-05-29
AI Technical Summary
In the existing chloromethyl ethyl ether production process, byproducts such as polychlorinated compounds and oligomers are difficult to remove, making it difficult for the product purity to exceed 95%. High-purity products required in high-end fields require complex post-processing processes, which also result in high production costs.
By employing a composite-specific catalyst, iron-calcium dual active sites are supported on a carbon fiber framework, allowing for precise control of the reaction pathway, reducing byproduct formation, and improving product purity.
It significantly improves the purity of chloromethyl ethyl ether, reduces production costs, conforms to the concept of green chemical industry, and the catalyst can be reused, reducing solid waste emissions.
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of chloromethyl ethyl ether technology, specifically a method for producing high-purity chloromethyl ethyl ether. Background Technology
[0002] Chloromethyl ethyl ether, as an important halogenated ether organic chemical intermediate, occupies a key position in the fine chemical industry due to its unique chloromethylation reactivity. Its core applications cover multiple fields, including pesticide synthesis (such as the preparation of intermediates for herbicides and insecticides), ion exchange resin synthesis (as a crosslinking agent and functionalizing reagent), pharmaceutical intermediate synthesis, and polymer material modification. It is also a commonly used reagent in the Blanc chloromethylation reaction and plays an irreplaceable role in the functionalization modification of aromatic derivatives, resulting in consistently stable market demand. As the pesticide, pharmaceutical, and polymer material industries upgrade towards high-end and refined products, more stringent requirements are being placed on the purity, stability, and environmental friendliness of chloromethyl ethyl ether products during production.
[0003] Currently, the industrial production of chloromethyl ethyl ether generally employs a liquid-phase process, using formaldehyde, ethanol, and hydrogen chloride as core raw materials in an addition-etherification reaction. Because formaldehyde is volatile at room temperature and has a low boiling point, directly using formaldehyde solution leads to high raw material loss and unstable reaction system concentration, not only reducing the yield of the target product but also causing environmental pollution and safety hazards due to formaldehyde escape. To address this issue, the industry commonly uses paraformaldehyde instead of formaldehyde solution as a reaction raw material. By utilizing the characteristic of paraformaldehyde to gradually depolymerize and release formaldehyde in the reaction system, formaldehyde volatilization is effectively suppressed, improving raw material utilization and reaction controllability, while also helping to increase the basic content of the product.
[0004] However, existing paraformaldehyde routes still face numerous technical bottlenecks, hindering the industrialization and upgrading of chloromethyl ethyl ether. From a reaction mechanism perspective, this process involves multiple cascaded reactions and parallel side reactions, resulting in a complex and interconnected reaction pathway: first, paraformaldehyde undergoes a stepwise depolymerization reaction under acidic conditions to generate free formaldehyde monomers; subsequently, formaldehyde undergoes an addition reaction with hydrogen chloride to form a chloromethyl cation intermediate, which then undergoes an etherification reaction with ethanol to generate the target product, chloromethyl ethyl ether. However, the chloromethyl cation intermediate is highly reactive and prone to multiple side reactions. Besides generating byproducts such as hydroxymethyl ethyl ether and various diethers, it also forms harmful impurities such as dichloromethyl ether and dichloromethyl ether. These byproducts have similar physicochemical properties to the target product and are difficult to completely remove using conventional separation methods. This results in the purity of existing industrial products generally failing to exceed 95%, and the high-purity products required in high-end applications rely on complex post-processing techniques, further increasing production costs. Summary of the Invention
[0005] The purpose of this invention is to provide a method for producing high-purity chloromethyl ethyl ether by adding a composite special catalyst to the production process, thereby precisely controlling the reaction path, significantly reducing the generation of by-products such as polychlorinated compounds and oligomers, and improving product purity.
[0006] The objective of this invention can be achieved through the following technical solutions: A method for producing high-purity chloromethyl ethyl ether includes the following steps: Step 1: Using styrene as a monomer, divinylbenzene as a crosslinking agent, isooctane as a pore-forming agent, and benzoyl peroxide as an initiator, a homogeneous precursor solution is obtained; carbon fibers are mixed with the precursor suspension, stirred to make the precursor uniformly coat the surface and gaps of the carbon fibers, rapidly shaped by liquid nitrogen freezing, and then calcined to obtain a carbon fiber skeleton.
[0007] Step 2: Sodium bicarbonate solution is fully penetrated into the pores of the carbon fiber skeleton. After adding calcium chloride solution, the two undergo a metathesis reaction in the skeleton pores. The resulting calcium carbonate nanoparticles are loaded in situ onto the skeleton pores and surface, thus obtaining a calcium-based carbon fiber skeleton.
[0008] Step 3: Using ethylene glycol as a solvent and complexing medium, sodium citrate and ferric chloride hexahydrate form a stable iron complex, which promotes the adsorption-complexation of the iron complex with calcium carbonate on the surface of the calcium-based framework, thus obtaining a composite special catalyst.
[0009] Step 4: Add anhydrous ethanol and paraformaldehyde with a mass fraction of 92-98% into the reactor, stir for 20-30 minutes at 15-25℃ and 500-600r / min, then add a composite special catalyst, and react with hydrogen chloride until the material becomes transparent. After sampling and analysis, separate the hydrochloric acid to obtain high-purity chloromethyl ethyl ether.
[0010] Furthermore, the mass ratio of anhydrous ethanol, paraformaldehyde, and the composite special catalyst is 1600-1700:1000-1200:0.8-1.5.
[0011] Furthermore, the specific steps for preparing the precursor solution are as follows: Styrene, divinylbenzene and deionized water are added to a reaction vessel and stirred for 20-30 min at 20-25℃ and 500-600 r / min. Then, isooctane as a porogen, benzoyl peroxide as an initiator and sodium dodecylbenzenesulfonate as a dispersant are added, and stirring is continued for 30-50 min to obtain a precursor solution.
[0012] Furthermore, the ratio of styrene, divinylbenzene, deionized water, isooctane, benzoyl peroxide, and sodium dodecylbenzenesulfonate is 20-22 kg: 15-18 kg: 80-90 L: 2-3 kg: 15-17 kg: 15-18 L.
[0013] Furthermore, the specific preparation steps of the carbon fiber skeleton are as follows: Carbon fibers with a length of 1-2 μm and a precursor solution are added to a reactor and stirred and dispersed at 50-60℃ and 500-600 r / min for 30-40 min. The mixture is then poured into a mold and frozen in liquid nitrogen for 10-12 min, followed by freeze-drying in a freeze dryer for 48-50 h. The mixture is then cut and transferred to a muffle furnace under nitrogen protection. It is heated to 350-370℃ at a rate of 5-6℃ / min and held for 2-4 h. Then, it is heated to 500-550℃ at a rate of 9-11℃ / min and held for 2-4 h. After natural cooling, the mixture is filtered, and the filter cake is washed 2-4 times with deionized water and vacuum dried at 60-80℃ for 1-2 h to obtain the carbon fiber skeleton.
[0014] Furthermore, the ratio of carbon fiber to precursor solution is 10⁻¹² kg: 10⁻¹² L.
[0015] Furthermore, the specific preparation steps of the calcium-based carbon fiber skeleton are as follows: A carbon fiber skeleton and a 10% sodium bicarbonate solution were added to a reaction vessel and vacuum impregnated for 2-3 hours at 20-25℃ and 500-600 r / min. Then, a 40-50% calcium chloride solution was added and the reaction was continued for 1-2 hours. The mixture was then filtered, and the filter cake was washed 2-4 times with deionized water and anhydrous ethanol, respectively. The mixture was then vacuum dried at 60-80℃ for 1-2 hours to obtain a calcium-based carbon fiber skeleton.
[0016] Furthermore, the ratio of carbon fiber skeleton, sodium bicarbonate solution, and calcium chloride solution is 10-12 kg: 30-32 L: 12-14 L.
[0017] Furthermore, the specific preparation steps for the composite-specific catalyst are as follows: Ferric chloride hexahydrate, sodium citrate, and ethylene glycol were added to a reactor and stirred for 20-30 minutes at 40-50℃ and 500-600 r / min. Then, sodium acetate and calcium-based carbon fiber skeleton were added, and the mixture was heated to 90-100℃ and stirred for 4-5 hours. After natural cooling, the mixture was filtered, and the filter cake was washed 2-4 times with deionized water and vacuum dried at 60-80℃ for 1-2 hours to obtain the composite special catalyst.
[0018] Furthermore, the mass ratio of ferric chloride hexahydrate, sodium citrate, ethylene glycol, sodium acetate, and calcium-based carbon fiber skeleton is 5-6:3-4:20-30:500-600:8-9.
[0019] The beneficial effects of this invention are: 1. The method for producing high-purity chloromethyl ethyl ether provided by the present invention incorporates a composite special catalyst into the production process, thereby precisely controlling the reaction path, significantly reducing the generation of by-products such as polychlorinated compounds and oligomers, and improving product purity.
[0020] 2. The composite catalyst prepared by this invention employs iron-calcium dual active sites to synergistically catalyze the chloromethylation reaction. The presence of dual sites results in high catalytic efficiency. The composite catalyst uses a carbon fiber skeleton as a support. The carbon fiber skeleton has a high specific surface area and porous structure. After calcium-based modification, the pores are evenly distributed, which not only achieves uniform loading of active components but also accelerates the diffusion and contact of reactants, promotes the full reaction, and further reduces impurity content. Furthermore, the carbon fiber skeleton has good mechanical stability, and can be quickly separated by filtration after the reaction. It can be reused after regeneration, reducing catalyst costs and solid waste emissions, which is in line with the concept of green chemical engineering. Detailed Implementation
[0021] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.
[0022] Example 1: A method for producing high-purity chloromethyl ethyl ether, comprising the following steps: S1: Add 20 kg of styrene, 15 kg of divinylbenzene and 80 L of deionized water to a reactor and stir for 20 min at 20 °C and 500 r / min. Then add 2 kg of isooctane as a porogen, 15 kg of benzoyl peroxide as an initiator and 15 L of sodium dodecylbenzenesulfonate as a dispersant. Continue stirring for 30 min to obtain the precursor solution.
[0023] S2: 10 kg of 1 μm long carbon fiber and 10 L of precursor solution were added to a reactor and stirred and dispersed at 50 °C and 500 r / min for 30 min. The mixture was poured into a mold and shaped, then frozen in liquid nitrogen for 10 min. It was then freeze-dried in a freeze dryer for 48 h, cut and shaped, transferred to a muffle furnace, protected with nitrogen, heated to 350 °C at a rate of 5 °C / min and held for 2 h, then heated to 500 °C at a rate of 9 °C / min and held for 2 h. After natural cooling, the mixture was filtered, and the filter cake was washed twice with deionized water and vacuum dried at 60 °C for 1 h to obtain the carbon fiber skeleton.
[0024] S3: Add 10 kg of carbon fiber skeleton and 30 L of 10% sodium bicarbonate solution to the reactor. Vacuum impregnate for 2 h at 20 °C and 500 r / min. Then add 12 L of 40% calcium chloride solution and continue the reaction for 1 h. Filter the mixture and wash the filter cake twice with deionized water and anhydrous ethanol, respectively. Dry the filter cake under vacuum at 60 °C for 1 h to obtain calcium-based carbon fiber skeleton.
[0025] S4: Add 5 kg of ferric chloride hexahydrate, 3 kg of sodium citrate, and 20 kg of ethylene glycol to a reactor and stir for 20 min at 40 °C and 500 r / min. Then add 500 g of sodium acetate and 8 kg of calcium-based carbon fiber skeleton, heat to 90 °C, continue stirring for 4 h, cool naturally, filter, wash the filter cake twice with deionized water, and vacuum dry at 60 °C for 1 h to obtain the composite special catalyst.
[0026] S5: Add 1600 kg of anhydrous ethanol and 1000 kg of 92% paraformaldehyde to a reactor, stir for 20 min at 15℃ and 500 r / min, then add 0.8 kg of composite special catalyst, and react with hydrogen chloride until the material becomes transparent. After sampling and analysis, hydrochloric acid is separated to obtain high-purity chloromethyl ethyl ether.
[0027] Example 2: A method for producing high-purity chloromethyl ethyl ether, comprising the following steps: S1: Add 21 kg of styrene, 16.5 kg of divinylbenzene and 85 L of deionized water to a reactor and stir for 25 min at 22.5 °C and 550 r / min. Then add 2.5 kg of isooctane as a porogen, 16 kg of benzoyl peroxide as an initiator and 16.5 L of sodium dodecylbenzenesulfonate as a dispersant. Continue stirring for 40 min to obtain the precursor solution.
[0028] S2: 11 kg of 1.5 μm long carbon fibers and 11 L of precursor solution were added to a reactor and stirred and dispersed at 55 °C and 550 r / min for 35 min. The mixture was poured into a mold and shaped, then frozen in liquid nitrogen for 11 min. It was then freeze-dried in a freeze dryer for 49 h, cut and shaped, and transferred to a muffle furnace. Nitrogen gas was introduced for protection, and the furnace was heated to 360 °C at a rate of 5.5 °C / min and held for 3 h. The furnace was then heated to 525 °C at a rate of 10 °C / min and held for 3 h. The mixture was allowed to cool naturally, filtered, and the filter cake was washed three times with deionized water and vacuum dried at 70 °C for 1.5 h to obtain the carbon fiber skeleton.
[0029] S3: 11 kg of carbon fiber skeleton and 31 L of 10% sodium bicarbonate solution were added to the reactor and impregnated under vacuum at 22.5 °C and 550 r / min for 2.5 h. Then, 13 L of 45% calcium chloride solution was added and the reaction was continued for 1.5 h. The mixture was filtered and the filter cake was washed three times with deionized water and anhydrous ethanol, respectively. The mixture was then dried under vacuum at 70 °C for 1.5 h to obtain calcium-based carbon fiber skeleton.
[0030] S4: Add 5.5 kg of ferric chloride hexahydrate, 3.5 kg of sodium citrate, and 25 kg of ethylene glycol to a reactor and stir for 25 min at 45 °C and 550 r / min. Then add 550 g of sodium acetate and 8.5 kg of calcium-based carbon fiber skeleton, heat to 95 °C, continue stirring for 4.5 h, cool naturally, filter, wash the filter cake three times with deionized water, and vacuum dry at 70 °C for 1.5 h to obtain the composite special catalyst.
[0031] S5: Add 1650 kg of anhydrous ethanol and 1100 kg of 95% paraformaldehyde to the reactor, stir for 25 min at 20℃ and 550 r / min, then add 1.15 kg of composite special catalyst, and react with hydrogen chloride until the material becomes transparent. After sampling and analysis, hydrochloric acid is separated to obtain high-purity chloromethyl ethyl ether.
[0032] Example 3: A method for producing high-purity chloromethyl ethyl ether, comprising the following steps: S1: Add 22 kg of styrene, 18 kg of divinylbenzene and 90 L of deionized water to a reactor and stir for 30 min at 25 °C and 600 r / min. Then add 3 kg of isooctane as a porogen, 17 kg of benzoyl peroxide as an initiator and 18 L of sodium dodecylbenzenesulfonate as a dispersant. Continue stirring for 50 min to obtain the precursor solution.
[0033] S2: 12 kg of 2 μm long carbon fibers and 12 L of precursor solution were added to a reactor and stirred and dispersed at 60 °C and 600 r / min for 40 min. The mixture was poured into a mold and shaped, then frozen in liquid nitrogen for 12 min. It was then freeze-dried in a freeze dryer for 50 h, cut and shaped, transferred to a muffle furnace, protected by nitrogen, heated to 370 °C at a rate of 6 °C / min and held for 4 h, then heated to 550 °C at a rate of 11 °C / min and held for 4 h. After natural cooling, the mixture was filtered, and the filter cake was washed 4 times with deionized water and vacuum dried at 80 °C for 2 h to obtain the carbon fiber skeleton.
[0034] S3: 12 kg of carbon fiber skeleton and 32 L of 10% sodium bicarbonate solution were added to the reactor and impregnated under vacuum at 25 °C and 600 r / min for 3 h. Then, 14 L of 50% calcium chloride solution was added and the reaction was continued for 2 h. The mixture was filtered and the filter cake was washed 4 times with deionized water and anhydrous ethanol, respectively. The mixture was then dried under vacuum at 80 °C for 2 h to obtain calcium-based carbon fiber skeleton.
[0035] S4: Add 6 kg of ferric chloride hexahydrate, 4 kg of sodium citrate, and 30 kg of ethylene glycol to a reactor and stir for 30 min at 50 °C and 600 r / min. Then add 600 g of sodium acetate and 9 kg of calcium-based carbon fiber skeleton, heat to 100 °C, continue stirring for 5 h, cool naturally, filter, wash the filter cake 4 times with deionized water, and vacuum dry at 80 °C for 2 h to obtain the composite special catalyst.
[0036] S5: Add 1700 kg of anhydrous ethanol and 1200 kg of 98% paraformaldehyde to a reactor, stir for 30 min at 25℃ and 600 r / min, then add 1.5 kg of composite special catalyst, and react with hydrogen chloride until the material becomes transparent. After sampling and analysis, hydrochloric acid is separated to obtain high-purity chloromethyl ethyl ether.
[0037] Comparative Example 1: Based on Example 3, the carbon fiber skeleton in step S3 is omitted.
[0038] Comparative Example 2: Based on Example 3, the composite special catalyst in step S5 was replaced with the calcium-based carbon fiber skeleton prepared in step S3.
[0039] Comparative Example 3: Based on Example 3, the calcium-based carbon fiber skeleton in step S4 was replaced with the carbon fiber skeleton prepared in step S2.
[0040] The purity and yield of chloromethyl ethyl ether obtained in Examples 1-3 and Comparative Examples 1-3 were tested, and the results are shown in Table 1: Table 1 As shown in Table 1, the yield in Comparative Example 1 dropped significantly to 62.3%. The original scheme exhibited a synergistic catalytic effect with its iron-calcium dual active sites; the calcium sites adsorbed and activated the aldehyde groups of paraformaldehyde, while the iron sites promoted bond breaking and formation in the chloromethylation reaction. Without the calcium sites, the activation efficiency of paraformaldehyde decreased, the reaction conversion rate dropped significantly, and the proportion of side reactions increased. Purity decreased; without the regulatory effect of the calcium sites, the reaction pathway became uncontrolled, generating a large amount of polychlorinated compounds, oligomers, and other impurities. Simultaneously, the pores of the pure carbon fiber skeleton lacked calcium modification, resulting in uneven pore distribution and hindered reactant diffusion, further exacerbating side reactions. Catalyst separation became more difficult: calcium modification can improve the hydrophilicity and mechanical stability of the support; without the calcium sites, the carbon fiber skeleton easily aggregated, reducing post-reaction filtration efficiency, and residual catalyst particles contaminated the product, further decreasing purity.
[0041] In Comparative Example 2, the yield decreased. The calcium-based carbon fiber skeleton could only adsorb and activate paraformaldehyde, failing to provide the catalytic active centers required for the chloromethylation reaction. The reaction relied solely on the spontaneous reaction of hydrogen chloride in the system, resulting in an extremely slow rate. A large amount of reactants remained unconverted, leading to a significantly lower yield than in the examples. Purity also decreased. Without precise control of iron sites, reaction selectivity was poor, and the amount of byproducts increased. However, because the calcium-based skeleton still possessed the ability to disperse impurities through pores, the purity reduction was slightly less than in Comparative Example 1. The reaction time was extended: the spontaneous reaction rate was much lower than that of the catalytic reaction, requiring a longer reaction time to achieve the aforementioned yield, significantly increasing the cost of industrial production.
[0042] In Comparative Example 3, the yield decreased. The unmodified carbon fiber skeleton had a low specific surface area and uneven pore distribution, making it prone to agglomeration of the iron active component after loading, resulting in a decrease in the exposure rate of active sites. Simultaneously, the lack of synergistic effect from calcium sites led to decreased catalytic efficiency, a lower yield than the example, and reduced purity. The uneven pore structure resulted in inconsistent reactant diffusion rates, with locally excessively high concentrations triggering side reactions. Furthermore, the carbon fiber skeleton lacked calcium-based impurity adsorption capacity, preventing some byproducts from being captured by the support, thus reducing product purity. The catalyst also exhibited poor reusability: the unmodified carbon fiber skeleton had weak mechanical stability, was easily damaged after the reaction, and had a high loss rate of active components, making regeneration impossible and inconsistent with green chemical engineering principles, increasing solid waste emissions and production costs.
[0043] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of the invention.
Claims
1. A method for producing high-purity chloromethyl ethyl ether, characterized in that, Includes the following steps: Step 1: Using styrene as a monomer, divinylbenzene as a crosslinking agent, isooctane as a pore-forming agent, and benzoyl peroxide as an initiator, a homogeneous precursor solution is obtained; carbon fibers are mixed with the precursor suspension, stirred to make the precursor uniformly coat the surface and gaps of the carbon fibers, rapidly shaped by liquid nitrogen freezing, and calcined to obtain a carbon fiber skeleton. Step 2: Sodium bicarbonate solution is fully penetrated into the pores of the carbon fiber skeleton. After adding calcium chloride solution, the two undergo a metathesis reaction in the pores of the skeleton. The resulting calcium carbonate nanoparticles are loaded in situ on the pores and surface of the skeleton to obtain a calcium-based carbon fiber skeleton. Step 3: Using ethylene glycol as a solvent and complexing medium, sodium citrate and ferric chloride hexahydrate form a stable iron complex, which promotes the adsorption-complexation of the iron complex with calcium carbonate on the surface of the calcium-based framework, thus obtaining a composite special catalyst. Step 4: Add anhydrous ethanol and paraformaldehyde with a mass fraction of 92-98% into the reactor, stir for 20-30 minutes at 15-25℃ and 500-600r / min, then add a composite special catalyst, and react with hydrogen chloride until the material becomes transparent. After sampling and analysis, separate the hydrochloric acid to obtain high-purity chloromethyl ethyl ether.
2. The method for producing high-purity chloromethyl ethyl ether according to claim 1, characterized in that, The mass ratio of anhydrous ethanol, paraformaldehyde, and the composite special catalyst is 1600-1700:1000-1200:0.8-1.
5.
3. The method for producing high-purity chloromethyl ethyl ether according to claim 1, characterized in that, The specific preparation steps of the precursor solution are as follows: Styrene, divinylbenzene and deionized water are added to a reaction vessel and stirred for 20-30 min at 20-25℃ and 500-600 r / min. Then, isooctane as a porogen, benzoyl peroxide as an initiator and sodium dodecylbenzenesulfonate as a dispersant are added, and stirring is continued for 30-50 min to obtain a precursor solution.
4. The method for producing high-purity chloromethyl ethyl ether according to claim 3, characterized in that, The ratio of styrene, divinylbenzene, deionized water, isooctane, benzoyl peroxide, and sodium dodecylbenzenesulfonate is 20-22 kg: 15-18 kg: 80-90 L: 2-3 kg: 15-17 kg: 15-18 L.
5. The method for producing high-purity chloromethyl ethyl ether according to claim 1, characterized in that, The specific preparation steps of the carbon fiber skeleton are as follows: Carbon fibers with a length of 1-2 μm and a precursor solution are added to a reactor and stirred and dispersed at 50-60℃ and 500-600 r / min for 30-40 min. The mixture is then poured into a mold and frozen in liquid nitrogen for 10-12 min, followed by freeze-drying in a freeze dryer for 48-50 h. The mixture is then cut and transferred to a muffle furnace under nitrogen protection. It is heated to 350-370℃ at a rate of 5-6℃ / min and held for 2-4 h. Then, it is heated to 500-550℃ at a rate of 9-11℃ / min and held for 2-4 h. After natural cooling, the mixture is filtered, and the filter cake is washed 2-4 times with deionized water and vacuum dried at 60-80℃ for 1-2 h to obtain the carbon fiber skeleton.
6. The method for producing high-purity chloromethyl ethyl ether according to claim 5, characterized in that, The ratio of carbon fiber to precursor solution is 10-12 kg: 10-12 L.
7. The method for producing high-purity chloromethyl ethyl ether according to claim 1, characterized in that, The specific preparation steps of the calcium-based carbon fiber skeleton are as follows: A carbon fiber skeleton and a 10% sodium bicarbonate solution were added to a reaction vessel and vacuum impregnated for 2-3 hours at 20-25℃ and 500-600 r / min. Then, a 40-50% calcium chloride solution was added and the reaction was continued for 1-2 hours. The mixture was then filtered, and the filter cake was washed 2-4 times with deionized water and anhydrous ethanol, respectively. The mixture was then vacuum dried at 60-80℃ for 1-2 hours to obtain a calcium-based carbon fiber skeleton.
8. The method for producing high-purity chloromethyl ethyl ether according to claim 7, characterized in that, The ratio of the carbon fiber skeleton, sodium bicarbonate solution, and calcium chloride solution is 10-12 kg: 30-32 L: 12-14 L.
9. The method for producing high-purity chloromethyl ethyl ether according to claim 1, characterized in that, The specific preparation steps of the composite catalyst are as follows: Ferric chloride hexahydrate, sodium citrate, and ethylene glycol were added to a reactor and stirred for 20-30 minutes at 40-50℃ and 500-600 r / min. Then, sodium acetate and calcium-based carbon fiber skeleton were added, and the mixture was heated to 90-100℃ and stirred for 4-5 hours. After natural cooling, the mixture was filtered, and the filter cake was washed 2-4 times with deionized water and vacuum dried at 60-80℃ for 1-2 hours to obtain the composite special catalyst.
10. The method for producing high-purity chloromethyl ethyl ether according to claim 9, characterized in that, The mass ratio of ferric chloride hexahydrate, sodium citrate, ethylene glycol, sodium acetate, and calcium-based carbon fiber skeleton is 5-6:3-4:20-30:500-600:8-9.