阅读说明：本技术 一种阴离子交换树脂的提纯工艺及提纯设备 (Purification process and purification equipment of anion exchange resin ) 是由 薛兆能 于 2020-11-06 设计创作，主要内容包括：本发明公开了一种阴离子交换树脂的提纯工艺及提纯设备,提纯工艺,包括以下步骤：使用氯化钠水溶液对阴离子交换树脂进行循环冲洗,得到氯化阴离子交换树脂；将氯化阴离子树脂使用碱性水溶液进行循环冲洗,然后将冲洗后的氯化阴离子树脂利用提纯设备进行气洗,然后得到一级阴离子交换树脂；将一级阴离子交换树脂使用亚硫酸钠溶液进行冲洗,然后再使用脱盐水进行冲洗,得到提纯的阴离子交换树脂,本发明克服了现有技术的不足,该工艺可有效的清除阴离子交换树脂内的大分子和阴离子,可在提纯设备内一次完成,不需要更换装置,节约了设备,简化了提纯操作工艺。(The invention discloses a purification process and purification equipment of anion exchange resin, wherein the purification process comprises the following steps: circularly washing the anion exchange resin by using a sodium chloride aqueous solution to obtain chlorinated anion exchange resin; circularly washing the chlorinated anion resin by using an alkaline aqueous solution, and then performing gas washing on the washed chlorinated anion resin by using purification equipment to obtain primary anion exchange resin; the invention overcomes the defects of the prior art, can effectively remove macromolecules and anions in the anion exchange resin, can be finished in a purifying device at one time, does not need to replace a device, saves the device, and simplifies the purifying operation process.)

1. A purification process of anion exchange resin is characterized by comprising the following steps:

s1, circularly washing the anion exchange resin by using a sodium chloride aqueous solution to obtain chlorinated anion exchange resin;

s2, circularly washing the chlorinated anion resin by using an alkaline aqueous solution, then carrying out gas washing on the washed chlorinated anion resin by using a purification device, and then obtaining primary anion exchange resin;

and S3, washing the primary anion exchange resin by using sodium sulfite solution, and then washing by using desalted water to obtain the purified anion exchange resin.

2. The process of claim 1, wherein the aqueous alkaline solution comprises sodium hydroxide, water, sodium salicylate, and sodium chloride.

3. The process of claim 1, wherein the gas washing comprises alternating water vapor washing and organic solvent vapor washing, wherein the organic solvent comprises ethylene diamine and ethanol.

4. The process of claim 3, wherein the steam washing uses steam containing ozone.

5. A purification equipment for anion exchange resin purification process according to claim 1, characterized in that, including purification tank and flushing tank, purification tank on be equipped with charge door and discharge gate, wherein the charge door is located purification tank's top, the discharge gate is located purification tank's lower part, purification tank's bottom still be equipped with the bin outlet, flushing tank install in purification tank's inside, and flushing tank's top and charge door be connected, the bottom is connected with the discharge gate, flushing tank not with purification tank contact, flushing tank be the jar body that the surface was equipped with a plurality of through-hole, charge door and discharge gate on all install sealing flange, and all install the rubber buffer in charge door and the discharge gate, purification tank's top be equipped with first inlet pipe, purification tank's left side be equipped with the second inlet pipe, flushing tank's internally mounted have the purification device, the purification device is communicated with the first feeding pipe and the second feeding pipe.

6. The purifying apparatus as claimed in claim 5, wherein the purifying device comprises a main pipe and a plurality of branch pipes disposed on the main pipe, the main pipe is vertically installed in the middle of the washing tank, the main pipe is closed at the bottom, the top of the main pipe is communicated with the first feeding pipe and the second feeding pipe, the branch pipes are divergently disposed on the main pipe and communicated with the main pipe, and the branch pipes are provided with a plurality of injection ports with upward openings.

7. The purifying apparatus as claimed in claim 6, wherein the injection port is circular, and a dividing portion integrally formed with the branch pipe is provided at a central portion of the injection port to divide the injection port into at least two portions.

8. The purifying apparatus of claim 7, wherein the partition has an inclined side surface and is inclined in a diverging manner from the inside of the branch tube.

Technical Field

The invention relates to the technical field of purification of anion exchange resin, and particularly belongs to a purification process and purification equipment of anion exchange resin.

Background

Ion exchange process is a reversible chemical reaction between ions in the liquid phase and ions in the solid phase, some of the ions in the liquid phase being adsorbed by the ion exchange solid to maintain the electrical neutrality of the aqueous solution, and the ion exchange solid must release the equivalent ions back into solution. The anion exchange resin is generally porous or granular, and has a size of about 0.1 to 1mm, and the ion exchange capacity thereof can be characterized by the following: strong base type anion exchange resin, weak base type anion exchange resin, adsorption to anion. When hydroxide anion resin contacts water to generate ion exchange reaction, various anions in water are adsorbed, and the water only contains one hydroxide ion. The adsorbed anions and organic molecules remain on or in the anion resin, so that the exchange capacity of the anions is gradually weakened, and at the moment, the anion exchange resin needs to be purified, purified and impurities removed, so that the adsorption capacity of the anion exchange resin is improved.

Disclosure of Invention

The invention aims to provide a purification process and purification equipment of anion exchange resin, which overcome the defects of the prior art.

In order to solve the problems, the technical scheme adopted by the invention is as follows:

a process for purifying an anion exchange resin comprising the steps of:

s1, circularly washing the anion exchange resin by using a sodium chloride aqueous solution to obtain chlorinated anion exchange resin;

s2, circularly washing the chlorinated anion resin by using an alkaline aqueous solution, then carrying out gas washing on the washed chlorinated anion resin by using a purification device, and then obtaining primary anion exchange resin;

and S3, washing the primary anion exchange resin by using sodium sulfite solution, and then washing by using desalted water to obtain the purified anion exchange resin.

Wherein the alkaline aqueous solution comprises sodium hydroxide, water, sodium salicylate and sodium chloride.

Wherein the gas washing comprises water vapor washing and organic solvent steam washing which are alternately carried out, wherein the organic solvent comprises ethylenediamine and ethanol, the pressure of the gas washing is 2-3Mpa, and the temperature is 70-90 ℃.

Wherein, the water vapor washing uses water vapor containing ozone.

The purifying equipment for the anion exchange resin purifying process comprises a purifying tank and a washing tank, wherein the purifying tank is provided with a feed inlet and a discharge outlet, wherein the charging opening is positioned at the top of the purifying tank, the discharging opening is positioned at the lower part of the purifying tank, the bottom of the purifying tank is also provided with a discharging opening, the flushing tank is arranged inside the purifying tank, the top of the washing tank is connected with the charging port, the bottom of the washing tank is connected with the discharging port, the washing tank is not contacted with the purifying tank, the washing tank is a tank body with a plurality of through holes on the surface, sealing flanges are arranged on the charging opening and the discharging opening, rubber plugs are arranged in the feed inlet and the discharge outlet, a first feed pipe is arranged at the top of the purification tank, the left side of purification jar be equipped with the second inlet pipe, the internally mounted of washing jar have the purification device, purification device and first inlet pipe and second inlet pipe intercommunication.

The purification device comprises a main pipe and a plurality of branch pipes arranged on the main pipe, the main pipe is vertically arranged in the middle of the flushing tank, the bottom of the main pipe is closed, the top of the main pipe is communicated with the first feeding pipe and the second feeding pipe, the branch pipes are divergently arranged on the main pipe and communicated with the main pipe, and the branch pipes are provided with a plurality of jet ports with upward openings.

The jet orifice is circular, and the middle part of the jet orifice is provided with a dividing part which is integrated with the branch pipe into a whole structure and divides the jet orifice into at least two parts.

The side surface of the dividing part is of an inclined structure and is inclined in a divergent manner from the inside of the branch pipe to the outside.

Compared with the prior art, the invention has the following implementation effects:

1. the invention utilizes the matching use of sodium salicylate and sodium hydroxide, so that in the process of replacing ions in the anion exchange resin by the sodium hydroxide, the salicylic acid radical can be complexed and combined with macromolecules combined in the pore canal of the anion exchange resin, and under the flushing action of alkaline aqueous solution, the macromolecules complexed with the salicylic acid radical are taken away, so that part of macromolecules and part of ions in the anion exchange resin are taken away from the pore canal of the anion exchange resin.

2. The invention uses the purification equipment to carry out air washing, leads water vapor to be flushed into the pore canal of the anion exchange resin through temperature and pressure, removes the residual and adsorbed ions and macromolecules in the anion exchange resin, increases the solubility of soluble substances through high temperature and high pressure, in addition, under the action of organic solvent steam, amino and hydroxyl in the ethylenediamine and the ethanol can be combined with anion exchange resin, so that residual ions in the anion exchange resin can be thoroughly removed, and simultaneously water vapor also contains ozone, under high temperature and high temperature, ozone can oxidize organic pollutants and macromolecules adsorbed in the anion resin, so that the organic pollutants and the macromolecules are degraded and can be taken away by ethanol in organic solvent steam, thereby effectively removing macromolecules and anions in the anion exchange resin after the gas washing.

3. The purification equipment can flush and gas-wash the anion exchange resin in the flushing tank, can realize multiple purposes in one tank, can complete the purification of the anion exchange resin in the tank body at one time, does not need to replace a device, saves the equipment and simplifies the purification operation.

4. When high-pressure steam is introduced into the main pipe of the purification device installed in the flushing tank, the dividing parts on the branch pipes are inclined in a divergent shape, so that the jet orifices of the branch pipes can form jet flows upwards, the anion exchange resin can be impacted, and simultaneously, under the simultaneous jetting action of the plurality of branch pipes on the main pipe, the anion exchange resin can be suspended and stirred, so that the anion exchange resin can be cleaned and purified in each direction under the jetting action, and the purification efficiency and effect are effectively improved.

Drawings

FIG. 1 is a schematic view of the inside of a purification apparatus;

FIG. 2 is a schematic structural view of a manifold;

fig. 3 is a sectional view of the injection port.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.

In the description of the present invention, it should be noted that the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation to be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.

In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; may be directly connected or indirectly connected through an intermediate. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.

Examples

As shown in fig. 1-3, the purification apparatus for anion exchange resin purification process comprises a purification tank 1 and a rinsing tank 7, wherein the purification tank 1 is provided with a feed inlet 11 and a discharge outlet 12, the feed inlet 11 and the discharge outlet 12 are both provided with sealing flanges 10, and rubber stoppers are respectively arranged in the feed inlet 11 and the discharge outlet 12 to seal the feed inlet 11 and the discharge outlet 12.

The charge door 11 is located the top of purification jar 1, discharge gate 12 is located the lower part of purification jar 1, the bottom of purification jar 1 still is equipped with bin outlet 15, wash jar 7 and install in the inside of purification jar 1, and wash the top of jar 7 and be connected with charge door 11, the bottom is connected with discharge gate 12, wash jar 7 not with purification jar 1 contact, wash jar 7 for the jar body that the surface is equipped with a plurality of through-hole, the top of purification jar 1 is equipped with first inlet pipe 13, the left side of purification jar 1 is equipped with second inlet pipe 14, the internally mounted of washing jar 7 has the purification device.

The purification device comprises a main pipe 8 and a plurality of branch pipes 9 arranged on the main pipe 8, the main pipe 8 is vertically arranged in the middle of a washing tank 7, the bottom of the main pipe 8 is closed, the top of the main pipe is communicated with a first feeding pipe 13 and a second feeding pipe 14, the branch pipes 9 are arranged on the main pipe 8 in a divergent shape and are communicated with the main pipe 8, a plurality of jet ports 91 with upward openings are arranged on the branch pipes 9, the jet ports 91 are circular, a dividing part 92 integrated with the branch pipes 9 is arranged in the middle of the jet ports 91, the jet ports 91 are divided into two parts, the side surfaces of the dividing part 92 are of inclined structures, and the inner parts of the branch pipes 9 are.

The organic content in the anion exchange resin before purification was 2240 mg/L. When the anion exchange resin is purified by using the purification equipment, firstly, 6 wt% of sodium chloride aqueous solution enters the main pipe 8 from the second feeding pipe 14, the first feeding pipe 13 is closed, the anion exchange resin is circularly washed by using the sodium chloride aqueous solution, the washed sodium chloride aqueous solution flows to the discharge port 15 at the bottom of the purification tank 1 from the space between the purification tank 1 and the washing tank 7, flows out from the discharge port 15, and is circularly washed for 20min, so that the chlorinated anion exchange resin is obtained;

then, the first feeding pipe 13 is continuously used for circularly washing the chlorinated anion resin by using an alkaline aqueous solution containing 3 wt% of sodium hydroxide, 1.2 wt% of sodium salicylate and 0.6 wt% of sodium chloride, then the first feeding pipe 13 is closed, and the washed chlorinated anion resin is subjected to gas washing by using a second feeding pipe 14, wherein the gas washing comprises water vapor washing and organic solvent steam washing which are alternately carried out, wherein the water vapor washing uses water vapor containing 4 wt% of ozone, the organic solvent steam is ethanol containing 8 wt% of ethylenediamine, the pressure of the gas washing is 3.0MPa, and the temperature is 80 ℃, and then the primary anion exchange resin is obtained.

Finally, the second feed line 14 was closed, and the primary anion exchange resin was washed with a 2.7 wt% sodium sulfite solution using the first feed line 13 to remove residual ozone and other oxidizing substances in the anion exchange resin, and then washed again with desalted water to obtain a purified anion exchange resin.

60mL of anion exchange resin purified by the method is detected, and the content of organic matters in the anion exchange resin is only 370 mg/L.

Comparative example 1

The difference from the example is that the alkali liquor does not contain sodium salicylate, 60mL of the purified anion exchange resin is taken, and the content of the organic matters in the anion exchange resin is only 1360mg/L through detection.

Comparative example 2

The difference from the example is that the water vapor does not contain ozone, 60mL of the purified anion exchange resin is taken, and the content of organic matters in the anion exchange resin is detected to be 1120 mg/L.

Comparative example 3

The difference from the example is that the organic solvent steam does not contain ethylenediamine, 60mL of the purified anion exchange resin is taken, and the content of organic matters in the anion exchange resin is only 980 mg/L.

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.