CN117049965A - Efficient recycling method for solvent in lithium salt additive production process - Google Patents
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- 239000002904 solvent Substances 0.000 title claims abstract description 55
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000000654 additive Substances 0.000 title claims abstract description 16
- 229910003002 lithium salt Inorganic materials 0.000 title claims abstract description 16
- 159000000002 lithium salts Chemical class 0.000 title claims abstract description 16
- 230000000996 additive effect Effects 0.000 title claims abstract 5
- 238000004064 recycling Methods 0.000 title abstract 2
- 238000004821 distillation Methods 0.000 claims abstract description 35
- 238000009835 boiling Methods 0.000 claims abstract description 30
- 239000002808 molecular sieve Substances 0.000 claims abstract description 18
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 150000002148 esters Chemical class 0.000 claims abstract description 11
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 11
- 239000012046 mixed solvent Substances 0.000 claims abstract description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 48
- 238000011084 recovery Methods 0.000 claims description 15
- 239000012528 membrane Substances 0.000 claims description 8
- -1 carbonate ester Chemical class 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 3
- 239000012141 concentrate Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 abstract 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 28
- 229910000029 sodium carbonate Inorganic materials 0.000 description 14
- 230000006872 improvement Effects 0.000 description 8
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical group ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- 230000018044 dehydration Effects 0.000 description 6
- 238000006297 dehydration reaction Methods 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 239000002000 Electrolyte additive Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical group COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/08—Purification; Separation; Stabilisation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/70—Compounds containing carbon and sulfur, e.g. thiophosgene
- C01B32/72—Carbon disulfide
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/84—Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/86—Separation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/6564—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms
- C07F9/6571—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms having phosphorus and oxygen atoms as the only ring hetero atoms
- C07F9/6574—Esters of oxyacids of phosphorus
- C07F9/65748—Esters of oxyacids of phosphorus the cyclic phosphorus atom belonging to more than one ring system
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
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Abstract
Description
技术领域Technical field
本发明涉及一种锂盐添加剂生产过程中溶剂的高效回收复用方法。The invention relates to an efficient recovery and reuse method of solvents in the production process of lithium salt additives.
背景技术Background technique
电解液作为锂离子电池4大主要组成部分，被称作锂离子电池的“血液”，其技术的发展是锂电池技术发展的关键环节。As the four main components of lithium-ion batteries, electrolyte is called the "blood" of lithium-ion batteries. The development of its technology is a key link in the development of lithium-ion battery technology.
二氟双草酸磷酸锂等作为电解液添加剂加入到锂离子电池电解液中，可以提高电池的耐高温和高电压性能，可以在正极材料表面形成稳定的固体电解质膜，提高电池循环性能。然而，在电解液添加剂生产过程中，需要使用大量的碳酸酯和低沸点溶剂等溶剂进行溶解及重结晶等操作。然而，现有技术中并没有如何对电解液添加剂生产过程中主要溶剂碳酸酯和低沸点溶剂回收及再利用的相关报道。Lithium difluorobisoxalate phosphate and the like are added as electrolyte additives to the lithium-ion battery electrolyte, which can improve the high temperature resistance and high voltage performance of the battery, form a stable solid electrolyte film on the surface of the cathode material, and improve the battery cycle performance. However, in the production process of electrolyte additives, a large amount of solvents such as carbonate esters and low-boiling point solvents need to be used for operations such as dissolution and recrystallization. However, there are no relevant reports in the prior art on how to recover and reuse the main solvent carbonate and low boiling point solvent in the production process of electrolyte additives.
发明内容Contents of the invention
本发明提供了一种锂盐添加剂生产过程中溶剂的高效回收复用方法，可以有效解决上述问题。The invention provides an efficient recovery and reuse method of solvents in the production process of lithium salt additives, which can effectively solve the above problems.
本发明是这样实现的：The invention is implemented as follows:
本发明提供一种锂盐添加剂生产过程中溶剂的高效回收复用方法，包括以下步骤：The invention provides a method for efficient recovery and reuse of solvents in the production process of lithium salt additives, which includes the following steps:
S1,从产线中回收碳酸酯和低沸点溶剂混合溶剂，在蒸馏浓缩装置中将温度设置在50~65℃进行蒸馏浓缩，其中，所述碳酸酯为沸点为70~100℃的低分子量碳酸酯；所述低沸点溶剂为沸点为0~50℃的低分子量低沸点溶剂；S1, recover the mixed solvent of carbonate and low-boiling point solvent from the production line, set the temperature in the distillation concentration device at 50~65°C for distillation and concentration, wherein the carbonate is low molecular weight carbonic acid with a boiling point of 70~100°C. Ester; the low-boiling-point solvent is a low-molecular-weight, low-boiling-point solvent with a boiling point of 0 to 50°C;
S2，将蒸馏浓缩后的碳酸酯进行脱酸,然后过滤；S2, deacidify the carbonate after distillation and concentration, and then filter;
S3，将过滤后的碳酸酯用所述蒸馏浓缩装置在105~120℃进行蒸馏浓缩，脱去金属离子；S3, use the distillation concentration device to distill and concentrate the filtered carbonate at 105~120°C to remove metal ions;
S4，将步骤S1中获得的低沸点溶剂及步骤S3中的碳酸酯分别使用分子筛进行脱水处理；S4, dehydrate the low boiling point solvent obtained in step S1 and the carbonate ester in step S3 using molecular sieves respectively;
S5，将脱水后的低沸点溶剂及碳酸酯分别过滤，分别得到净化后的碳酸酯和低沸点溶剂返回产线中复用S5, filter the dehydrated low-boiling-point solvent and carbonate respectively, and obtain the purified carbonate and low-boiling-point solvent respectively and return them to the production line for reuse.
本发明的有益效果是：本发明提供的锂盐添加剂生产过程中溶剂的高效回收复用方法，通过上述步骤可以实现主要溶剂碳酸酯和低沸点溶剂的回收及再利用，从而大大节约生产成本，且使整个产生实现绿色可循环。The beneficial effects of the present invention are: the efficient recovery and reuse method of solvents in the production process of lithium salt additives provided by the present invention can realize the recovery and reuse of main solvent carbonate and low boiling point solvent through the above steps, thus greatly saving production costs. And make the entire production green and recyclable.
附图说明Description of the drawings
为了更清楚地说明本发明实施方式的技术方案，下面将对实施方式中所需要使用的附图作简单地介绍，应当理解，以下附图仅示出了本发明的某些实施例，因此不应被看作是对范围的限定，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他相关的附图。In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show certain embodiments of the present invention and therefore do not It should be regarded as a limitation of the scope. For those of ordinary skill in the art, other relevant drawings can be obtained based on these drawings without exerting creative efforts.
图1是本发明实施例提供的锂盐添加剂生产过程中溶剂的高效回收复用方法的流程图。Figure 1 is a flow chart of a method for efficient recovery and reuse of solvents in the production process of lithium salt additives provided by an embodiment of the present invention.
具体实施方式Detailed ways
为使本发明实施方式的目的、技术方案和优点更加清楚，下面将结合本发明实施方式中的附图，对本发明实施方式中的技术方案进行清楚、完整地描述，显然，所描述的实施方式是本发明一部分实施方式，而不是全部的实施方式。基于本发明中的实施方式，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施方式，都属于本发明保护的范围。因此，以下对在附图中提供的本发明的实施方式的详细描述并非旨在限制要求保护的本发明的范围，而是仅仅表示本发明的选定实施方式。基于本发明中的实施方式，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施方式，都属于本发明保护的范围。In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments These are some embodiments of the present invention, but 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 efforts fall within the scope of protection of the present invention. Accordingly, the following detailed description of embodiments of the invention provided in the appended drawings is not intended to limit the scope of the claimed invention, but rather to represent selected embodiments of the invention. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts fall within the scope of protection of the present invention.
在本发明的描述中，术语“第一”、“第二”仅用于描述目的，而不能理解为指示或暗示相对重要性或者隐含指明所指示的技术特征的数量。由此，限定有“第一”、“第二”的特征可以明示或者隐含地包括一个或者更多个该特征。在本发明的描述中，“多个”的含义是两个或两个以上，除非另有明确具体的限定。In the description of the present invention, the terms "first" and "second" are used for descriptive purposes only and cannot be understood as indicating or implying relative importance or implicitly indicating the number of indicated technical features. Therefore, features defined as "first" and "second" may explicitly or implicitly include one or more of these features. In the description of the present invention, "plurality" means two or more than two, unless otherwise explicitly and specifically limited.
参照图1所示，本发明实施例提供一种锂盐添加剂生产过程中溶剂的高效回收复用方法，包括以下步骤：Referring to Figure 1, an embodiment of the present invention provides a method for efficient recovery and reuse of solvents in the production process of lithium salt additives, which includes the following steps:
S1,从产线中回收碳酸酯和低沸点溶剂混合溶剂，在蒸馏浓缩装置中将温度设置在50~65℃进行蒸馏浓缩，其中，所述碳酸酯为沸点为70~100℃的低分子量碳酸酯；所述低沸点溶剂为沸点为0~50℃的低分子量低沸点溶剂；S1, recover the mixed solvent of carbonate and low-boiling point solvent from the production line, set the temperature in the distillation concentration device at 50~65°C for distillation and concentration, wherein the carbonate is low molecular weight carbonic acid with a boiling point of 70~100°C. Ester; the low-boiling-point solvent is a low-molecular-weight, low-boiling-point solvent with a boiling point of 0 to 50°C;
S2，将蒸馏浓缩后的碳酸酯进行脱酸,然后过滤；S2, deacidify the carbonate after distillation and concentration, and then filter;
S3，将过滤后的碳酸酯用所述蒸馏浓缩装置在105~120℃进行蒸馏浓缩，脱去金属离子；S3, use the distillation concentration device to distill and concentrate the filtered carbonate at 105~120°C to remove metal ions;
S4，将步骤S1中获得的低沸点溶剂及步骤S3中的碳酸酯分别使用分子筛进行脱水处理；S4, dehydrate the low boiling point solvent obtained in step S1 and the carbonate ester in step S3 using molecular sieves respectively;
S5，将脱水后的低沸点溶剂及碳酸酯分别过滤，分别得到净化后的碳酸酯和低沸点溶剂返回产线中复用。S5: Filter the dehydrated low-boiling-point solvent and carbonate respectively, and obtain the purified carbonate and low-boiling-point solvent respectively and return them to the production line for reuse.
在其中一个实施例中，所述碳酸酯选自碳酸二甲酯。所述低沸点溶剂选自卤代烷烃、醚类、醇类及腈类等，在其中多个实施例中，所述低沸点溶剂分别为二氯甲烷、乙醚、二甲胺、二硫化碳 。试验证明，当蒸馏浓缩的温度过低，会显著增加蒸馏浓缩的时间，当蒸馏浓缩温度过高，会使低沸点溶剂中混有碳酸酯溶剂。作为进一步改进的，在步骤S1中，所述在蒸馏浓缩装置中将温度设置在50~65℃进行蒸馏浓缩的步骤具体包括：In one embodiment, the carbonate is selected from dimethyl carbonate. The low boiling point solvent is selected from halogenated alkanes, ethers, alcohols, nitriles, etc. In many embodiments, the low boiling point solvent is methylene chloride, diethyl ether, dimethylamine, and carbon disulfide. Tests have shown that when the temperature of distillation and concentration is too low, the time of distillation and concentration will be significantly increased. When the temperature of distillation and concentration is too high, carbonate solvents will be mixed with low-boiling point solvents. As a further improvement, in step S1, the step of setting the temperature in the distillation concentration device at 50~65°C for distillation and concentration specifically includes:
在蒸馏浓缩装置中将温度设置在54~60℃进行蒸馏浓缩。在其中一个实施例中，在蒸馏浓缩装置中将温度设置在56℃进行蒸馏浓缩（碳酸酯选自碳酸二甲酯、所述低沸点溶剂为二氯甲烷）。Set the temperature in the distillation concentration device at 54~60°C for distillation and concentration. In one embodiment, the temperature in the distillation concentration device is set to 56°C for distillation and concentration (the carbonate is selected from dimethyl carbonate, and the low-boiling point solvent is dichloromethane).
作为进一步改进的，在步骤S2中，所述将蒸馏浓缩后的碳酸酯进行脱酸的步骤具体包括：As a further improvement, in step S2, the step of deacidifying the distilled and concentrated carbonate specifically includes:
将蒸馏浓缩后的碳酸酯加入Na2CO3进行脱酸处理。使用碳酸钠进行脱酸的原因是，一方面，碳酸钠不溶于碳酸酯，且其本身是碱性物质，和酸会发生反应生成不溶于碳酸酯的盐而沉淀下来，而不会产生额外的杂质；另一方面，碳酸钠本身具有一定的吸水性能，可以预先对碳酸酯进行第一步的脱水，降低后续吸附剂的负担。定义加入Na2CO3进行脱酸处理的碳酸钠的理论总摩尔数为Xmol,其中，所述理论总摩尔数为通过需处理的碳酸酯的总量及其含酸量计算获得。为了将酸性完全中和，且进行预脱水，优选的，实际加入进行脱酸处理的碳酸钠摩尔数为B，其中，2.5X≧B≧2.2X。在其中一个实施例中，实际加入进行脱酸处理的碳酸钠摩尔数B=2.3X。试验证明，当实际加入进行脱酸处理的碳酸钠为理论添加量的2.3倍左右时，不仅仅可以实现脱酸，还可以实现良好的预脱水（预脱水中的水的来源有两部分，一部分是中和反应产生的水，另一部分是碳酸酯本身自带的水）。Add Na 2 CO 3 to the distilled and concentrated carbonate for deacidification. The reason for using sodium carbonate for deacidification is that, on the one hand, sodium carbonate is insoluble in carbonate and is an alkaline substance. It will react with acid to form a salt that is insoluble in carbonate and precipitate without producing additional salts. impurities; on the other hand, sodium carbonate itself has certain water absorption properties, which can pre-dehydrate the carbonate in the first step and reduce the burden on the subsequent adsorbent. The theoretical total number of moles of sodium carbonate added to Na 2 CO 3 for deacidification treatment is defined as In order to completely neutralize the acidity and perform pre-dehydration, it is preferred that the number of moles of sodium carbonate actually added for deacidification treatment is B, where 2.5X≧B≧2.2X. In one of the embodiments, the actual number of moles of sodium carbonate added for deacidification treatment was B=2.3X. Tests have proven that when the actual amount of sodium carbonate added for deacidification is about 2.3 times the theoretical amount, not only deacidification can be achieved, but also good pre-dehydration can be achieved (the source of water in pre-dehydration has two parts, one part It is the water produced by the neutralization reaction, and the other part is the water contained in the carbonate itself).
本发明将60升pH值为0.1mol/L、含水率(体积)约为2.4%的碳酸二甲酯溶液，等分为6份（其中X约为0.5mol），通过不同含量的碳酸钠进行处理后的结果进行比较如下表1所示：In the present invention, 60 liters of dimethyl carbonate solution with a pH value of 0.1mol/L and a moisture content (volume) of approximately 2.4% is divided into 6 equal parts (where The processed results are compared as shown in Table 1 below:
表1为碳酸酯溶液经过不同含量的碳酸钠进行处理后的含水率表Table 1 shows the moisture content of the carbonate solution after being treated with different contents of sodium carbonate.
从上述表格中可以看出，当加入理论量的1.5倍的碳酸钠时，其含水率变化不明显，这是由于使用碳酸钠进行脱酸，其本身会产生一定的水份，因此，如果没有足量的碳酸钠进行脱水。其含水率不仅不会产生太大变化，还会增加，即起不到预脱水作用。进一步的，当碳酸钠加入到理论加入量的2.3倍时，继续添加碳酸钠其产生的脱水效果不会产生太大变化。由此可见，最优的添加量为理论的2.3倍左右。It can be seen from the above table that when 1.5 times the theoretical amount of sodium carbonate is added, the change in moisture content is not obvious. This is because the use of sodium carbonate for deacidification will produce a certain amount of moisture. Therefore, if there is no Sufficient sodium carbonate for dehydration. Not only will its moisture content not change much, it will also increase, that is, it will not play a pre-dehydration role. Furthermore, when sodium carbonate is added to 2.3 times the theoretical amount, the dehydration effect produced by continuing to add sodium carbonate will not change much. It can be seen that the optimal addition amount is about 2.3 times the theoretical amount.
作为进一步改进的，在步骤S2中，脱酸后，可经过精密过滤器对碳酸酯进行过滤，以去除反应后的盐沉淀及剩余的碳酸钠固体。As a further improvement, in step S2, after deacidification, the carbonate can be filtered through a precision filter to remove salt precipitates and remaining sodium carbonate solids after the reaction.
作为进一步改进的，在步骤S3中，所述将过滤后的碳酸酯用所述蒸馏浓缩装置在105~115℃进行蒸馏浓缩，脱去金属离子的步骤包括：As a further improvement, in step S3, the filtered carbonate is distilled and concentrated using the distillation concentration device at 105~115°C, and the step of removing metal ions includes:
将过滤后的碳酸酯用所述蒸馏浓缩装置在108~115℃进行蒸馏浓缩，脱去金属离子。通过这一步骤，可以将碳酸酯中部分与金属离子形成络合物或配合物的碳酸酯分子与金属离子分离，从而脱去金属离子。The filtered carbonate is distilled and concentrated using the distillation concentration device at 108~115°C to remove metal ions. Through this step, some carbonate molecules that form complexes or complexes with metal ions in the carbonate can be separated from the metal ions, thereby removing the metal ions.
作为进一步改进的，在步骤S4中，将步骤S1中获得的低沸点溶剂使用分子筛进行脱水处理的步骤：As a further improvement, in step S4, the low boiling point solvent obtained in step S1 is dehydrated using molecular sieves:
将步骤S1中获得的低沸点溶剂使用4A分子筛进行脱水处理。The low boiling point solvent obtained in step S1 is dehydrated using 4A molecular sieve.
作为进一步改进的，在步骤S4中，将步骤S3中的碳酸酯使用分子筛进行脱水处理的步骤：As a further improvement, in step S4, the carbonate in step S3 is dehydrated using molecular sieves:
将步骤S3中的碳酸酯使用NaA型分子筛膜进行脱水处理。The carbonate in step S3 is dehydrated using a NaA molecular sieve membrane.
作为进一步改进的，所述将步骤S3中的碳酸酯使用NaA型分子筛膜进行脱水处理后，还进一步包括：As a further improvement, after the carbonate in step S3 is dehydrated using a NaA molecular sieve membrane, the method further includes:
将步骤S3中的碳酸酯使用NaA型分子筛膜进行脱水处理后取样检测水分，水分合格返回产线中复用，水分不合格在NaA型分子筛膜中多次循环；使最终的碳酸酯的纯度可以达到99.9%以上。The carbonate in step S3 is dehydrated using a NaA molecular sieve membrane and then sampled to detect the moisture. If the moisture is qualified, it is returned to the production line for reuse. If the moisture is unqualified, it is circulated in the NaA molecular sieve membrane multiple times; so that the purity of the final carbonate can be Reaching more than 99.9%.
以上所述仅为本发明的优选实施方式而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention and are not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and changes. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention shall be included in the protection scope of the present invention.
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