阅读说明：本技术 一种多元醇副产粗甲酸钠的纯化方法 (Purification method of crude sodium formate as byproduct of polyol ) 是由 慈敦锋 于 2019-09-18 设计创作，主要内容包括：本发明公开了一种多元醇副产粗甲酸钠的纯化方法,包括步骤1：将多元醇及副产粗甲酸钠加入反应釜中,缓慢添加乙酸乙酯溶液,并且使用交流电动机带动搅拌棒在反应釜中对混合溶液进行匀速搅拌,则粗甲酸钠溶解在乙酸乙酯溶液内,步骤2：将溶液放入蒸馏器皿中,对蒸馏器皿进行加热,然后采用冷凝水对蒸馏器皿加热的蒸汽进行冷凝,在预期甲酸钠到达沸点之前有沸点较低的液体先行蒸出,本发明涉及纯化方法技术领域。该多元醇副产粗甲酸钠的纯化方法,因为流动的冷凝水能够始终保持低温的状态,可以适当的提高冷凝速度,并且通过在获取稳定的甲酸钠前对不稳定的甲酸钠溶液进行接收清除,大大的提高了甲酸钠的的纯度。(The invention discloses a purification method of crude sodium formate as a byproduct of polyol, which comprises the following steps of 1: adding the polyhydric alcohol and the byproduct crude sodium formate into a reaction kettle, slowly adding an ethyl acetate solution, and driving a stirring rod to stir the mixed solution in the reaction kettle at a constant speed by using an alternating current motor, so that the crude sodium formate is dissolved in the ethyl acetate solution, and the step 2: the solution is put into a distillation vessel, the distillation vessel is heated, then steam heated by the distillation vessel is condensed by condensed water, and liquid with lower boiling point is distilled out before the expected sodium formate reaches the boiling point. According to the purification method of the crude sodium formate as the byproduct of the polyol, the flowing condensed water can be always kept in a low-temperature state, so that the condensation speed can be properly increased, and the unstable sodium formate solution is received and removed before stable sodium formate is obtained, so that the purity of the sodium formate is greatly increased.)

1. A purification method of crude sodium formate as a byproduct of polyol is characterized by comprising the following steps:

step 1: adding the polyhydric alcohol and the byproduct crude sodium formate into a reaction kettle, slowly adding an ethyl acetate solution, and driving a stirring rod to stir the mixed solution in the reaction kettle at a constant speed by using an alternating current motor, so that the crude sodium formate is dissolved in the ethyl acetate solution;

step 2: putting the solution into a distillation vessel, heating the distillation vessel, condensing steam heated by the distillation vessel by using condensed water, wherein the flow speed of the condensed water is proper, the liquid with lower boiling point is firstly distilled out before the expected sodium formate reaches the boiling point, the front fraction is collected into a plurality of drops through a test tube, and after the front fraction is discarded, a receiving bottle is replaced to collect the residual pure product;

and step 3: when the distillation amount of the sodium formate solution is less, a Kjeldahl head and a round-bottom flask are adopted, water vapor is poured into the bottom of a distillation flask through a glass tube, a drop of turbid liquid is condensed and accumulated in a receiving bottle along with hot vapor in the process of steam distillation, and the distilled liquid is clarified after all the distilled substances are evaporated;

and 4, step 4: when the boiling point difference between the sodium formate solution and the impurities is small, a fractionating column connected with the distillation flask and the distillation head generates a stable temperature difference, and at the moment, the related operations in the step 2 can be repeated to separate substances;

and 5: when the step 4 is operated, inert materials are added into the column, so that the surface area is increased, and the fractionation speed is accelerated;

step 6: pouring the separated sodium formate into a filtering membrane, and allowing the waste liquid to pass through the filtering membrane, so that the sodium formate is remained on the surface of the filtering membrane;

and 7: pouring sodium formate on the surface of the filtering membrane into a sodium chloride solution, and taking the sodium formate out of the solution after cleaning;

and 8: putting the taken sodium formate into a granular drying agent box, then putting the granular drying agent box into a stirring rod pair to roll, adding the granular drying agent into the drying agent box in batches, and continuously rolling the added sodium formate;

and step 9: the dried sodium formate was removed and the desiccant particles were filtered.

2. The method for purifying crude sodium formate as a byproduct from polyol production according to claim 1, wherein: in the step 1, the alternating current motor is driven by commercial power.

3. The method for purifying crude sodium formate as a byproduct from polyol production according to claim 1, wherein: in the step 2, an alcohol lamp is adopted to heat the distillation vessel.

4. The method for purifying crude sodium formate as a byproduct from polyol production according to claim 1, wherein: in the step 3, the round-bottom flask is 5L in specification. .

5. The method for purifying crude sodium formate as a byproduct from polyol production according to claim 1, wherein: in the step 5, the inert materials in the device are glass, ceramics and metal sheets.

6. The method for purifying crude sodium formate as a byproduct from polyol production according to claim 1, wherein: in the step 6, the filtering membrane can allow the solution to pass through but not allow sodium formate to pass through.

7. The method for purifying crude sodium formate as a byproduct from polyol production according to claim 1, wherein: in the step 7, the radius of the granular drying agent is 1-2 mm.

Technical Field

The invention relates to the technical field of purification methods, in particular to a purification method of crude sodium formate as a byproduct of polyol.

Background

Alcohols are a large class of organic compounds, and are compounds in which a hydrogen atom in a side chain of an aliphatic hydrocarbon, alicyclic hydrocarbon or aromatic hydrocarbon is substituted with a hydroxyl group. Alcohol, which is broadly defined in the general sense, refers to a compound having a hydroxyl group bonded to an aliphatic hydrocarbon group; hydroxyl groups are attached to benzene rings and are classified as phenols because they are chemically different from ordinary alcohols; hydroxyl is connected with hybridized double-bond carbon atom, belongs to enol, most of the compounds can not exist stably because the compounds can be tautomeric into ketone, and polyhydric alcohol is alcohol containing two or more hydroxyl in the molecule. The polyhydric alcohol is generally dissolved in water, and most of the polyhydric alcohols have viscous liquid or crystalline solid with the characteristics of high boiling point, strong dissolving capacity for polar substances, low toxicity and volatility and the like. The boiling point, viscosity, relative density, melting point, etc. increase with increasing molecular weight. Sodium formate is also known as sodium formate, and the crystals contain two crystal waters, thus sodium formate dihydrate, and sodium formate dihydrate. Sodium formate is the simplest organic carboxylate, either as a white crystal or powder, with a slight formic acid odor, which decomposes to hydrogen gas and sodium oxalate upon heating, with the subsequent formation of sodium carbonate. Sodium formate is mainly used for producing sodium hydrosulfite, oxalic acid and formic acid. In leather industry, as camouflage acid in chrome tanning, as a catalyst and stabilizer for synthesis, as a reducing agent in the printing and dyeing industry. Sodium formate is harmless to human body, and has irritation effect on eyes, respiratory system and skin.

In the traditional polyol production and experimental processes, a large amount of sodium formate which is an accessory product of polyol is obtained, but the purity of the sodium formate which is an accessory product of the polyol is low, the sodium formate cannot be applied in production and life, the traditional extraction mode is usually direct distillation, but impurities are excessive in the distillation process, and the purification efficiency is low.

Disclosure of Invention

Technical problem to be solved

Aiming at the defects of the prior art, the invention provides a purification method of crude sodium formate as a byproduct of polyol, which solves the problems that the purity of the concomitant product sodium formate is low and cannot be applied in production and life, and the traditional extraction mode is usually direct distillation, but the impurities in the early production stage are excessive and the purification efficiency is low.

(II) technical scheme

In order to achieve the purpose, the invention is realized by the following technical scheme: a purification method of crude sodium formate as a byproduct of polyol comprises the following steps:

step 1: adding the polyhydric alcohol and the byproduct crude sodium formate into a reaction kettle, slowly adding an ethyl acetate solution, and driving a stirring rod to stir the mixed solution in the reaction kettle at a constant speed by using an alternating current motor, so that the crude sodium formate is dissolved in the ethyl acetate solution;

step 2: putting the solution into a distillation vessel, heating the distillation vessel, condensing steam heated by the distillation vessel by using condensed water, wherein the flow speed of the condensed water is proper, the liquid with lower boiling point is firstly distilled out before the expected sodium formate reaches the boiling point, the front fraction is collected into a plurality of drops through a test tube, and after the front fraction is discarded, a receiving bottle is replaced to collect the residual pure product;

and step 3: when the distillation amount of the sodium formate solution is less, a Kjeldahl head and a round-bottom flask are adopted, water vapor is poured into the bottom of a distillation flask through a glass tube, a drop of turbid liquid is condensed and accumulated in a receiving bottle along with hot vapor in the process of steam distillation, and the distilled liquid is clarified after all the distilled substances are evaporated;

and 4, step 4: when the boiling point difference between the sodium formate solution and the impurities is small, a fractionating column connected with the distillation flask and the distillation head generates a stable temperature difference, and at the moment, the related operations in the step 2 can be repeated to separate substances;

and 5: when the step 4 is operated, inert materials are added into the column, so that the surface area is increased, and the fractionation speed is accelerated;

step 6: pouring the separated sodium formate into a filtering membrane, and allowing the waste liquid to pass through the filtering membrane, so that the sodium formate is remained on the surface of the filtering membrane;

and 7: pouring sodium formate on the surface of the filtering membrane into a sodium chloride solution, and taking the sodium formate out of the solution after cleaning;

and 8: putting the taken sodium formate into a granular drying agent box, then putting the granular drying agent box into a stirring rod pair to roll, adding the granular drying agent into the drying agent box in batches, and continuously rolling the added sodium formate;

and step 9: the dried sodium formate was removed and the desiccant particles were filtered.

Preferably, in step 1, the ac motor is driven by the commercial power.

Preferably, in the step 2, the distillation vessel is heated by an alcohol lamp.

Preferably, in the step 3, the round-bottom flask is 5L in specification.

Preferably, in the step 5, the inert materials in the device are glass, ceramic and metal sheets.

Preferably, in the step 6, the filtering membrane can allow the solution to pass through but not allow sodium formate to pass through.

Preferably, in the step 7, the radius of the granular drying agent is 1-2 mm.

(III) advantageous effects

The invention provides a purification method of a polyol by-product crude sodium formate. Compared with the prior art, the method has the following beneficial effects:

(1) the purification method of the crude sodium formate as the byproduct of the polyol comprises the steps of putting a solution into a distillation vessel, heating the distillation vessel, condensing steam heated by the distillation vessel by adopting condensed water, wherein the flowing speed of the condensed water is proper, the liquid with a lower boiling point is evaporated before the expected sodium formate reaches the boiling point, collecting a plurality of drops of the former fraction through a test tube, discarding the collected residual pure product, replacing a receiving bottle to collect the residual pure product, introducing the condensed water with a proper flow speed during the distillation of the sodium formate, wherein the flowing condensed water can be always kept in a low-temperature state, the condensing speed can be properly improved, and the unstable sodium formate solution is received and removed before the stable sodium formate is obtained, so that the purity of the sodium formate is greatly improved, the problem that the product sodium formate is low in purity and cannot be applied in production and life is solved, the traditional extraction method is usually to directly carry out distillation, but the problem that the purification efficiency is low due to excessive impurities in the distillation process is solved.

(2) The purification method of the crude sodium formate as the byproduct of the polyol comprises the steps of adopting a Kjeldahl head and a round-bottom flask when the distillation amount of a sodium formate solution is small, pouring water vapor into the bottom of a distillation flask through a glass tube, condensing and gathering a drop of turbid liquid along with hot steam in a steam distillation process in a receiving bottle, clarifying the distilled liquid after all distilled substances are evaporated, generating stable temperature difference by a fractionating column connected with the distillation flask and the distillation head when the boiling point difference of the sodium formate solution and impurities is small, repeating the related operation and material separation in the step 2, and using the Kjeldahl head and the round-bottom flask in a matching way to ensure that all the distilled substances can be evaporated even if the distillation amount of the sodium formate solution is small in the steam distillation process, effectively improving the conversion efficiency of distillation, generating the temperature difference by the fractionating column connected with the distillation flask and the distillation head, the distillation effect when the boiling point difference between the sodium formate solution and the impurity is small can be effectively improved.

(3) The purification method of the coarse sodium formate as the byproduct of the polyol comprises the steps of pouring precipitated sodium formate into a filtering membrane, enabling waste liquid to pass through the filtering membrane, keeping the sodium formate on the surface of the filtering membrane, putting the taken sodium formate into a granular drying agent box, rolling the sodium formate in the drying agent box through a stirring rod, adding the sodium formate into the drying agent box in batches, continuously rolling the added sodium formate, filtering liquid impurities on the surface of the sodium formate effectively through the filtering membrane, and effectively removing the moisture on the surface of the sodium formate through the arrangement of granular drying agents in the drying box, so that the dryness of the sodium formate is guaranteed, and the purification conversion rate of the sodium formate is effectively improved.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The embodiment of the invention provides a technical scheme that: a purification method of crude sodium formate as a byproduct of polyol comprises the following steps:

step 1: adding the polyhydric alcohol and the byproduct crude sodium formate into a reaction kettle, slowly adding an ethyl acetate solution, and driving a stirring rod to stir the mixed solution in the reaction kettle at a constant speed by using an alternating current motor, so that the crude sodium formate is dissolved in the ethyl acetate solution;

step 2: putting the solution into a distillation vessel, heating the distillation vessel, condensing steam heated by the distillation vessel by using condensed water, wherein the flow speed of the condensed water is proper, the liquid with lower boiling point is firstly distilled out before the expected sodium formate reaches the boiling point, the front fraction is collected into a plurality of drops through a test tube, after the front fraction is discarded, a receiving bottle is replaced to collect the residual pure product, the receiving bottle is prepared during transfer, and the receiving bottle can be directly replaced without waiting or interrupting the operation;

and step 3: when the distillation amount of the sodium formate solution is less, a Kjeldahl head and a round-bottom flask are adopted, water vapor is poured into the bottom of a distillation flask through a glass tube, a drop of turbid liquid is condensed and accumulated in a receiving bottle along with hot vapor in the process of steam distillation, and the distilled liquid is clarified after all the distilled substances are evaporated;

and 4, step 4: when the boiling point difference between the sodium formate solution and the impurities is small, a fractionating column connected with the distillation flask and the distillation head generates a stable temperature difference, and at the moment, the related operations in the step 2 can be repeated to separate substances;

and 5: when the step 4 is operated, inert materials are added into the column, so that the surface area is increased, and the fractionation speed is accelerated;

step 6: pouring the separated sodium formate into a filtering membrane, and allowing the waste liquid to pass through the filtering membrane, so that the sodium formate is remained on the surface of the filtering membrane;

and 7: pouring sodium formate on the surface of the filtering membrane into a sodium chloride solution, and taking the sodium formate out of the solution after cleaning to obtain high-purity sodium formate;

and 8: putting the taken sodium formate into a granular drying agent box, then putting the granular drying agent box into a stirring rod pair to roll, adding the granular drying agent into the drying agent box in batches, and continuously rolling the added sodium formate;

and step 9: the dried sodium formate was removed and the desiccant particles were filtered.

In step 1, an alternating current motor is driven by mains supply, condensed water with proper flow rate is introduced during sodium formate distillation, the flowing condensed water can be kept in a low-temperature state all the time, the condensation speed can be properly improved, and unstable sodium formate solution is received and removed before stable sodium formate is obtained, so that the purity of sodium formate is greatly improved, the problems that the purity of the sodium formate accompanying the product is low and cannot be applied in production and life are solved, the traditional extraction mode is usually direct distillation, but impurities are excessive in the early production stage and the purification efficiency is low are solved, in step 2, an alcohol lamp is adopted to heat a distillation vessel, and the distilled product can be completely evaporated by adopting the matching of a Kjeldahl head and a round-bottom flask, so that in the steam distillation process, even if the distillation quantity of the sodium formate solution is small, the distillation conversion efficiency is effectively improved, the temperature difference is generated by the flow dividing column connected with the distillation head through the distillation flask, the distillation effect when the boiling point difference between a sodium formate solution and impurities is small can be effectively improved, in the step 3, the round-bottom flask is in a 5L specification, liquid impurities on the surface of the sodium formate can be effectively filtered through the filtering membrane, in addition, through the arrangement of the granular drying agent in the drying box, the moisture on the surface of the sodium formate can be effectively removed, the dryness of the sodium formate is ensured, the purification conversion rate of the sodium formate is effectively improved, in the step 5, inert materials in the device are glass, ceramics and metal sheets, in the step 6, the filtering membrane can enable the solution to pass through the forbidden sodium formate, in the step 7, the radius of the granular drying agent is 1-.

It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.