阅读说明：本技术 一种电子级异丙醇的生产系统 (Production system of electronic grade isopropanol ) 是由 冯烈 许京伟 陈云斌 刘尚文 孙斌 孙琪 于 2020-04-21 设计创作，主要内容包括：本发明涉及电子级异丙醇的制造技术领域,针对异丙醇制备过程工艺步骤繁琐的问题,公开了一种电子级异丙醇的生产系统,包括原料输送单元、分子筛吸附单元、蒸发罐、第一精馏单元、第二精馏单元及过滤单元,上述设备之间依次连接,所述分子筛吸附单元内设有改性吸附材料,所述第一精馏单元内设有第一精馏填料区,第二精馏单元内侧的进口与出口之间设有第二精馏填料区,所述原料输送单元还设有进料口A,所述过滤单元还设有出料口B。本发明制备过程采用一步法脱水,采用具有磁性定向吸附能力及超大比表面能的改性吸附材料,最终得到异丙醇纯度较高及金属离子含量较低的电子级异丙醇,且制备得到能优异稳定的电子级异丙醇,生产工艺简但高效。(The invention relates to the technical field of manufacturing of electronic grade isopropanol, and discloses a production system of electronic grade isopropanol aiming at the problem of complicated process steps in the preparation process of isopropanol. The preparation process adopts a one-step method for dehydration, adopts a modified adsorption material with magnetic directional adsorption capacity and ultra-large specific surface energy, finally obtains the electronic grade isopropanol with higher purity and lower metal ion content, and prepares the electronic grade isopropanol with excellent and stable performance, and the production process is simple and efficient.)

1. The utility model provides a production system of electronic grade isopropanol, its characterized in that includes raw materials conveying unit (1), molecular sieve adsorption unit (2), evaporating pot (3), first rectification unit (4), second rectification unit (5) and filter unit (6), connects gradually between the above-mentioned equipment, be equipped with modified adsorption material in molecular sieve adsorption unit (2), be equipped with first rectification filler district (4.1) in first rectification unit (4), be equipped with second rectification filler district (5.1) between the import and the export of second rectification unit (5) inboard, raw materials conveying unit (1) still is equipped with feed inlet A, filter unit (6) still is equipped with discharge gate B.

2. The electronic grade isopropanol production system according to claim 1, wherein a circulation unit (7) is arranged outside the second rectification unit (5), one end of the circulation unit (7) is connected to the bottom of the second rectification unit (5), and the other end of the circulation unit (7) is connected between the second rectification packing region (5.1) and the outlet of the second rectification unit (5).

3. The electronic grade isopropanol production system of claim 1, wherein the modified adsorption material is permanent-magnet hydroxypropyl chitosan modified activated carbon, and the preparation method comprises:

(1) activated carbon activation: adding activated carbon into deionized water at 50-80 deg.C, ultrasonic treating for 0.5-1h, activating in 10-15% nitric acid solution for 20-30min, and washing with deionized water;

(2) preparing magnetic hydroxypropyl chitosan gel: placing hydroxypropyl chitosan in a container, adding acetic acid with the mass fraction of 4-6%, heating in water bath at 30-40 ℃ for 30-40min while mechanically stirring at 850-plus-900 rpm, adding 3, 5-dimethyl-2-pyrrole formaldehyde into the solution, raising the temperature to 65-70 ℃ at 2-4 ℃/min, stirring at 1200-plus-1500 rpm at constant temperature for 6-7h, and adding Fe plus to the solution₃O₄Rare earth magnet nanoparticles are stirred at the normal temperature of 800-;

(3) grafting activated carbon: adding 3-triethoxysilyl-1-propylamine into the product obtained in the step (1), heating to 30-40 ℃, and reacting for 20-40min for later use;

(4) preparing magnetic hydroxypropyl chitosan modified activated carbon: adding the product in the step (2) into the activated carbon grafted in the step (3), uniformly stirring, adding glyoxal glycidyl ether, heating to 40-50 ℃, keeping the temperature, stirring at 1000-1200rpm for 20-30min, then dripping into 0.8-1.2mol/L NaOH solution to form black gel beads, washing with deionized water, drying the gel beads in a 50-60 ℃ oven for 20-22h, and grinding to obtain magnetic powder;

(5) permanent magnetic treatment: and (4) magnetizing the magnetic powder in the step (4) and performing permanent magnetization treatment to obtain a finished product.

4. The system for producing electronic grade isopropanol according to claim 3, wherein the hydroxypropyl chitosan preparation process in step (2) comprises: uniformly mixing chitosan, 35-45% by mass of sodium hydroxide and propylene oxide according to the mass ratio of 1:1-1.2:14-15, carrying out alkalization treatment at 4-8 ℃ for 24-28h, heating to 40-50 ℃ and reacting for 7-9h to obtain hydroxypropyl chitosan.

5. The system for producing electronic grade isopropanol according to claim 3, wherein in step (2), the hydroxypropyl chitosan, 3, 5-dimethyl-2-pyrrolecarboxaldehyde and Fe₃O₄-the amount of rare earth magnet nanoparticles added is 1:0.8-1: 0.6-0.8.

6. The system for producing electronic grade isopropanol according to claim 3, wherein the amount of acetic acid added in step (2) is 8-10 times that of hydroxypropyl chitosan.

7. The electronic grade isopropanol production system of claim 3, wherein the mass ratio of hydroxypropyl chitosan to glyoxal glycidyl ether in step (4) is 1: 0.2-0.4.

8. The system for producing electronic grade isopropanol as claimed in claim 3, wherein the mass ratio of activated carbon to 3-triethoxysilyl-1-propylamine in step (3) is 1: 2-3.

9. The electronic grade isopropanol production system of claim 3,fe in step (2)₃O₄-the method of preparing rare earth magnet nanoparticles comprises: mixing Fe₃O₄Uniformly mixing the nano particles with strontium, barium and Nd elements to obtain mixed permanent magnetic powder, then placing the mixed permanent magnetic powder into calcining equipment, uniformly heating the mixed permanent magnetic powder to 400-plus-one temperature of 600 ℃ for heat preservation for 1-2h under vacuum or inert atmosphere, and preserving the heat for 2-4h after 800-plus-one temperature of 1000 ℃ to obtain Fe₃O₄-rare earth magnet nanoparticles.

10. The electronic grade isopropanol production system of claim 9, wherein Fe is₃O₄The input mass ratio of the nano particles to the strontium, barium and Nd is respectively 10-12: 1-2: 1-2: 0.5-1.

Technical Field

The invention relates to the technical field of manufacturing of electronic-grade isopropanol, in particular to a production system of electronic-grade isopropanol.

Background

Isopropanol is an organic compound, an isomer of n-propanol, known as dimethyl methanol, 2-propanol, also known in the industry as IPA. Isopropanol is an important chemical product and raw material. The method is mainly used for pharmacy, cosmetics, plastics, spices, coatings and the like, and various isopropanol purification processes have been reported at home and abroad, and the purification method mainly comprises the following steps: the method comprises the following steps: the purification method comprises the steps of decolorization, adsorption and rectification, or the combination of decolorization, adsorption and rectification, and the like, and has the defects of low product purity, unsatisfied scientific research requirements, low yield, high cost and the like. Therefore, a need exists for a low-cost process for producing isopropanol that produces pure isopropanol at a high yield and a high quality, and that significantly reduces the level of impurities such as dust and moisture in the final isopropanol product.

The invention discloses a preparation method of high-purity isopropanol with patent number CN201210434323.2, and relates to a preparation method of high-purity isopropanol, which takes industrial-grade isopropanol as a raw material, and sequentially and continuously purifies to obtain the high-purity isopropanol according to the steps of molecular sieve dehydration, resin dehydration, reverse osmosis, high-temperature rectification, ion exchange and circulating filtration. The purification route of the invention is reasonably and skillfully designed, and finally the high-quality electronic grade isopropanol with each single cation concentration less than 10ppt, each single anion concentration less than 1ppb and moisture content less than 20ppm can be obtained, and the stable and reliable batch and large-scale production of the electronic grade isopropanol can be realized.

The method has the disadvantages that the molecular sieve and resin are required to be dehydrated in multiple steps, reverse osmosis and other processes are also required, and the preparation process has low efficiency and high energy consumption.

Disclosure of Invention

The invention aims to overcome the problems of complicated process steps and high energy consumption of equipment in the isopropanol preparation process in the prior art, and provides an electronic grade isopropanol production system, which is a manufacturing system with high impurity adsorption efficiency.

In order to achieve the purpose, the invention adopts the following technical scheme:

the utility model provides a production system of electronic grade isopropanol, includes that raw materials carries unit, molecular sieve adsorption element, evaporating pot, first rectification unit, second rectification unit and filter unit, connects gradually between the above-mentioned equipment, be equipped with modified adsorption material in the molecular sieve adsorption element, be equipped with first rectification filler district in the first rectification unit, be equipped with second rectification filler district between the inboard import of second rectification unit and the export, raw materials carries the unit still to be equipped with feed inlet A, filter unit still is equipped with discharge gate B.

Raw material isopropanol is introduced into the raw material conveying unit from the feed inlet A, sequentially flows through the molecular sieve adsorption unit, the evaporation tank, the first rectifying unit, the second rectifying unit and the filtering unit, and finally isopropanol with higher purity is prepared at the filtering unit; the molecular sieve dehydration unit mainly adopts multi-stage molecular sieve adsorption to remove the water in the raw material isopropanol to below 30 ppm; the two-stage rectification mainly adopts stainless steel packed towers with different polishing grades to remove light components and metal ions in the isopropanol, so that the metal ions reach below 10 ppt; and finally, enabling the electronic grade isopropanol to meet the requirements of the production process through a filtering unit.

The modified adsorption material is arranged in the adsorption unit, has a large specific surface area, can adsorb small impurity particles and has a strong adsorption effect on metal ions, so that the isopropanol flowing through the modified adsorption material has high purity, the complexity in the subsequent treatment steps is greatly reduced, the number of times of isopropanol cyclic treatment is reduced, the energy loss of equipment is remarkably reduced, and the preparation efficiency of the isopropanol is greatly improved.

Preferably, a circulating unit is arranged outside the second rectifying unit, one end of the circulating unit is connected with the bottom of the second rectifying unit, and the other end of the circulating unit is connected between the second rectifying packing area and the outlet of the second rectifying unit.

The second rectifying unit is arranged behind the first rectifying unit and is used for absorbing the ultrapure isopropanol from the first rectifying unit to obtain electronic-grade isopropanol; the circulation loop is provided with a circulation unit which can remove impurities introduced in the absorption tower or in the circulation process, and the circulation loop is also provided with a condensing unit which is used for cooling the whole circulation system so as to control the temperature of the whole circulation system to be constant and prevent the temperature of the system from being too high, and finally the electronic grade isopropanol is obtained through the filtering unit, so that the purity of the final product is improved.

Preferably, the system for producing electronic grade isopropanol according to claim 1, wherein the modified adsorbent material is permanent-magnetic hydroxypropyl chitosan modified activated carbon, and the preparation method comprises:

(1) activated carbon activation: adding activated carbon into deionized water at 50-80 deg.C, ultrasonic treating for 0.5-1h, activating in 10-15% nitric acid solution for 20-30min, and washing with deionized water;

(2) preparing magnetic hydroxypropyl chitosan gel: placing hydroxypropyl chitosan in a container, adding acetic acid with the mass fraction of 4-6%, heating in water bath at 30-40 ℃ for 30-40min while mechanically stirring at 850-plus-900 rpm, adding 3, 5-dimethyl-2-pyrrole formaldehyde into the solution, raising the temperature to 65-70 ℃ at 2-4 ℃/min, stirring at 1200-plus-1500 rpm at constant temperature for 6-7h, and adding Fe plus to the solution₃O₄Rare earth magnet nanoparticles are stirred at the normal temperature of 800-;

(3) grafting activated carbon: adding 3-triethoxysilyl-1-propylamine into the product obtained in the step (1), heating to 30-40 ℃, and reacting for 20-40min for later use;

(4) preparing magnetic hydroxypropyl chitosan modified activated carbon: adding the product in the step (2) into the activated carbon grafted in the step (3), uniformly stirring, adding glyoxal glycidyl ether, heating to 40-50 ℃, keeping the temperature, stirring at 1000-1200rpm for 20-30min, then dripping into 0.8-1.2mol/L NaOH solution to form black gel beads, washing with deionized water, drying the gel beads in a 50-60 ℃ oven for 20-22h, and grinding to obtain magnetic powder;

(5) permanent magnetic treatment: and (4) magnetizing the magnetic powder in the step (4) and performing permanent magnetization treatment to obtain a finished product.

The active carbon has the advantages that the active carbon has aperture independence and easy adsorption saturation, and limited impurities and metals adsorbed by the active carbon are easy to be partially desorbed after saturation;

the hydroxypropyl chitosan molecular chain contains rich amino and hydroxyl and has stronger crosslinking capacity, so that the final material has stronger integrity by combining the hydroxypropyl chitosan with a connecting body of a magnetic material and active carbon, but the hydroxypropyl chitosan has poor mechanical property and reduces the adsorption performance of the hydroxypropyl chitosan to heavy metals, therefore, other functional groups such as pyrrole groups with aromatic conjugate rings containing N hetero atoms are introduced into the chitosan molecular chain in the step (2), so that the hydroxypropyl chitosan has stronger electron supply performance and coordination capacity, and is introduced into the hydroxypropyl chitosan molecular chain, so that the adsorption performance of the chitosan to the heavy metals can be greatly improved, in addition, two methyl groups are introduced, more active reaction sites are increased, the substitution degree on the main chain of macromolecules is further improved, the steric hindrance effect on the main chain is improved, and the positive promotion effect is played for increasing the crosslinking degree of the hydroxypropyl chitosan, the moisture absorption and retention of the fabric can be further improved;

the magnetic hydroxypropyl chitosan gel is prepared from hydroxypropyl chitosan and Fe₃O₄-rare earth magnet nanoparticles of Fe₃O₄The magnetic hydroxypropyl chitosan adsorption material prepared by combining the rare earth magnet nanoparticles and the chitosan has the advantages of being porous, large in specific surface area, narrow in particle size distribution and the like, and the overall adsorption capacity, stability and application value of the activated carbon material are effectively improved;

activating the activated carbon in the step (1) to improve active groups such as hydroxyl and other functional groups on the surface of the activated carbon, and performing the step (2) on Fe₃O₄Carrying out crosslinking reaction on rare earth magnet nano particles and hydroxypropyl chitosan introduced with pyrrolyl to prepare Fe₃O₄The preparation method comprises the following steps of (1) grafting activated carbon on magnetic hydroxypropyl chitosan gel solution with uniformly distributed rare earth magnet nanoparticles, providing a stable bridge effect for the close combination of the activated carbon and the magnetic hydroxypropyl chitosan gel solution by introducing a polyamino structure into the activated carbon in the step (3), and magnetizing the magnetic powder in the step (5) to ensure that Fe in the material is uniform₃O₄The rare earth magnet nanoparticles are magnetic, and finally the whole permanent magnet hydroxypropyl shell modified activated carbon is magnetic. The adsorbed object contains negatively charged acid radical ions such as chloride ions, carbonate ions and the like besides metal ions, and the permanent magnet hydroxypropyl shell poly-modified activated carbon has large adsorption specific surface area, also has magnetic force and has better effect on metal ions and anionsThe adsorption effect of (2) and the magnetic attraction force between the permanent-magnet hydroxypropyl shell modified activated carbon powder, so that the clearance between the permanent-magnet hydroxypropyl shell modified activated carbon powder is reduced, the modified adsorption material powder is more compact, and the purification and dehumidification performance of the isopropanol are better when the isopropanol passes through the modified adsorption material.

In conclusion, the modified adsorbing material has stronger purification effect and moisture absorption and retention performance on the isopropanol, reduces the circulation frequency of the isopropanol, and shortens the preparation period of the isopropanol.

Preferably, the preparation process of hydroxypropyl chitosan in step (2) comprises the following steps: mixing chitosan, 35-45% by mass of sodium hydroxide and propylene oxide according to the mass ratio of 1:1-1.2:14-15, performing alkalization treatment for 24-28h at 4-8 ℃, and heating to 40-50 ℃ for reaction for 7-9h to obtain hydroxypropyl chitosan.

The chitosan molecular chain has abundant amino and hydroxyl groups and stronger crosslinking capacity, so that the chitosan serving as a connecting body of the magnetic material and the activated carbon can enable the final material to have stronger integrity, but the chitosan has the defects of poor mechanical property, poor solubility, poor water solubility and the like, and the application range of the chitosan is limited.

Preferably, the 3, 5-dimethyl-2-pyrrolecarboxaldehyde and Fe are used in the step (2)₃O₄-the rare earth magnet nanoparticles are added in an amount of 1:0.8-1: 0.6-0.8.

Preferably, the addition amount of the acetic acid in the step (2) is 8-10 times of that of hydroxypropyl chitin.

The acetic acid is added to dissolve and disperse the hydroxypropyl chitosan in the solution, so that the uniform dispersibility of the hydroxypropyl chitosan solution is better.

Preferably, the mass ratio of hydroxypropyl chitosan to glyoxal glycidyl ether in the step (4) is 1: 0.2-0.4.

Introduction of a crosslinking agent glyoxal glycidyl ether such thatFurther crosslinking reaction of-NH 2 or-OH on hydroxypropyl chitosan macromolecular chain to obtain stable reticular crosslinked polymer with intertwined molecules. The cross-linked polymer has more stable chemical structure, is not easy to dissolve in a medium, has improved adsorption performance on pollutants, smaller swelling degree and higher recoverability, and has higher cross-linked mesh density and higher Fe content after the cross-linking degree of macromolecular chains is increased₃O₄Better coating of rare earth magnet nanoparticles, Fe₃O₄The stability of the rare earth magnet nanoparticles in the hydroxypropyl chitosan cross-linked network is higher, the rare earth magnet nanoparticles are not easy to fall off in the liquid impact washing process, and the overall stability of the adsorbing material is better.

Preferably, the mass ratio of the activated carbon to the 3-triethoxysilyl-1-propylamine in the step (3) is 1: 2-3.

The 3-triethoxysilyl-1-propylamine has a polyamino structure, amino on the polyamino structure can react with hydroxyl on the surface of the activated carbon and also can react with active groups on the magnetic hydroxypropyl chitosan gel solution, and the structure is a better reaction group bridging structure, so that the finally prepared modified adsorption material has higher integrity and stronger compactness.

Preferably, Fe in step (2)₃O₄-the method of preparing rare earth magnet nanoparticles comprises: mixing Fe₃O₄Uniformly mixing the nano particles with strontium, barium and Nd elements to obtain mixed permanent magnetic powder, then placing the mixed permanent magnetic powder into calcining equipment, uniformly heating the mixed permanent magnetic powder to 400-plus-one temperature of 600 ℃ for heat preservation for 1-2h under vacuum or inert atmosphere, and preserving the heat for 2-4h after 800-plus-one temperature of 1000 ℃ to obtain Fe₃O₄-rare earth magnet nanoparticles.

Preferably, Fe₃O₄The input mass ratio of the nano particles to the strontium, barium and Nd is respectively 10-12: 1-2: 1-2: 0.5-1.

The adoption of the sectional calcination can ensure the uniformity and stability inside and outside the permanent magnetic powder, and the gradual optimization of the physical and chemical properties is gradually realized.

Therefore, the invention has the following beneficial effects:

(1) the electronic grade isopropanol production system is provided, the manufacturing system with high impurity adsorption efficiency is prepared, in addition, the molecular sieve adsorption system has better moisture absorption and retention performance and excellent water removal effect, and finally the electronic grade isopropanol with higher isopropanol quality purity and lower metal ion content is obtained;

(2) the permanent-magnetic hydroxypropyl shell modified activated carbon has large adsorption specific surface area energy and magnetic force, has a good directional adsorption effect on metal ions, and meanwhile, the modified adsorption materials attract each other, so that the modified adsorption material powder is more compact, and the purification efficiency of isopropanol is high;

(3) the preparation process of the isopropanol is simple, the standard of one-step dehydration is realized, the equipment energy consumption is low, the preparation period is short, and the electronic grade isopropanol with excellent and stable performance can be finally prepared.

Drawings

FIG. 1 is a schematic view of a process flow of an isopropanol production system according to the present invention.

In the figure: 1. the device comprises a raw material conveying unit, 2 a molecular sieve adsorption unit, 3 an evaporation tank, 4 a first rectification unit, 4.1 a first rectification packing area, 5 a second rectification unit, 5.1 a second rectification packing area, 6 a filtering unit, 7 and a circulation unit.

Detailed Description

The invention is further described with reference to specific embodiments.