Purification device for electronic-grade polycarboxylic acid product

Abstract

The utility model relates to the technical field of separation and purification, in particular to a purification device for an electronic-grade polycarboxylic acid product. The utility model adopts the following technical scheme that the device comprises an anion exchange column, a cation exchange column and a stirring kettle, an anion exchange liquid inlet is formed in the upper part of the anion exchange column, and an anion exchange liquid outlet is formed in the bottom of the anion exchange column; the anion exchange liquid inlet is connected with an industrial-grade polycarboxylic acid aqueous solution conveying pipeline through a pipeline and is connected with a valve, an electronic flowmeter and a transmission pump in series; a cation exchange liquid inlet is formed in the upper part of the cation exchange column, a cation exchange liquid outlet is formed in the bottom of the cation exchange column, and the cation exchange liquid inlet is connected with the cation exchange liquid outlet of the anion exchange column through a pipeline and is connected with a valve, an electronic flowmeter and a transmission pump in series. According to the utility model, the electronic-grade polycarboxylic acid aqueous solution is produced in a continuous feeding and continuous discharging manner, so that the production efficiency is improved, and the production cost is reduced; the exchange efficiency of the cationic resin is improved, and the resin usage amount of a unit product is saved.

Description

TECHNICAL FIELD

[0001] The utility model relates to the technical field of separation, purification, especially relates to a kind of purification device of electronic grade polycarboxylic acid product. BACKGROUND

[0002] Electronic grade polycarboxylic acid is a cleaning agent for high-end precision devices such as electronic components, and the purity and metal ion content are very high, usually produced by purification using industrial grade polycarboxylic acid. The types of metal ions contained in the polycarboxylic acid produced industrially are diverse, and the content is mostly PPM level. The anion is mostly sulfate ion. Anion exchange resin is generally used to remove sulfate, and cation exchange resin is used to remove various metal ions, so that the ion content reaches PPB level.

[0003] Dynamic adsorption is usually used in industry to remove various metal ions. The low adsorption rate of dynamic adsorption resin will result in high consumption of cation resin. If static adsorption is used to improve the adsorption rate of resin, the production cycle will be prolonged due to the doubling of adsorption time. SUMMARY

[0004] To solve the problems in the prior art, the present application provides a purification device for electronic grade polycarboxylic acid product, which can effectively reduce the amount of cation resin used and continuously produce electronic grade polycarboxylic acid aqueous solution.

[0005] To achieve the above-mentioned purpose, the utility model adopts the following technical scheme:

[0006] The purification device for electronic grade polycarboxylic acid product of the utility model comprises an anion exchange column, a cation exchange column and a stirring kettle. The upper part of the anion exchange column is provided with an anion exchange inlet, and the bottom is provided with an anion exchange outlet. The anion exchange inlet is connected to the industrial grade polycarboxylic acid aqueous solution conveying pipeline through a pipeline and is connected in series with a valve, an electronic flowmeter and a transfer pump.

[0007] The upper part of the cation exchange column is provided with a cation exchange inlet, and the bottom is provided with a cation exchange outlet. The cation exchange inlet is connected to the cation exchange outlet of the anion exchange column through a pipeline and is connected in series with a valve, an electronic flowmeter and a transfer pump.

[0008] The top of the stirring kettle is provided with a stirring inlet and a stirring resin inlet, the bottom is provided with a stirring outlet, the outer wall is provided with a stirring constant-temperature heat exchanger. The stirring inlet is connected to the cation exchange column and the electronic grade polycarboxylic acid conveying pipeline through a three-way joint. The stirring resin inlet is connected to the resin weighing tank through a pipeline and is connected in series with a valve. The stirring outlet is connected to the electronic grade polycarboxylic acid conveying pipeline through a pipeline and is connected in series with a valve, an electronic flowmeter and a suction filter pump.

[0009] According to the electronic grade polycarboxylic acid product purification device, the anion exchange column and the cation exchange column are both cylindrical, the cross section inner diameter is 3-10cm, and the length-diameter ratio is (20-30):1.

[0010] According to the electronic grade polycarboxylic acid product purification device, the left end of the tee is connected with the cation exchange outlet through a pipeline and is connected with a valve in series; the upper end is connected with the stirring inlet through a pipeline and is connected with a valve, an electronic flow meter and a transmission pump in series; and the right end is connected with the electronic grade polycarboxylic acid transmission pipeline through a pipeline and is connected with a valve, an electronic flow meter and a transmission pump in series.

[0011] According to the electronic grade polycarboxylic acid product purification device, the anion exchange column, the cation exchange column and the stirring kettle can be connected in parallel according to actual needs, and N is greater than or equal to 2.

[0012] According to the electronic grade polycarboxylic acid product purification device, the cross section inner diameter of the anion exchange column and the cation exchange column is 5cm, and the length is 1.2m, and two groups are connected in parallel.

[0013] According to the electronic grade polycarboxylic acid product purification device, the stirring kettle is a 2000L enamel kettle, and two are connected in parallel.

[0014] According to the electronic grade polycarboxylic acid product purification device, the anion exchange resin uses OH type anion exchange resin, the cation exchange resin uses hydrogen type cation exchange resin, and the anion exchange resin and the cation exchange resin are spherical particles with a diameter of about 1-2mm.

[0015] The electronic grade polycarboxylic acid product purification device provided by the utility model produces electronic grade polycarboxylic acid aqueous solution in a continuous feeding and discharging mode, improves production efficiency and reduces production cost; meanwhile, the device effectively improves the exchange efficiency of cation resin, saves the resin usage amount of unit product, further reduces resin regeneration cost and is beneficial to industrial promotion. ACCURACY OF DRAWINGS

[0016] Figure 1 It is a whole structure schematic view of the utility model

[0017] In the drawing: 1, anion exchange column, 101, anion exchange inlet, 102, anion exchange outlet, 2, cation exchange column, 201, cation exchange inlet, 202, cation exchange outlet, 3, stirring kettle, 301, stirring inlet, 302, stirring resin inlet, 303, stirring outlet, 304, stirring constant temperature heat exchanger, 4, tee. DETAILED DESCRIPTION

[0018] The utility model will be further described in detail in combination with the drawings and specific embodiments.

[0019] The utility model discloses electronic grade polycarboxylic acid product's purification device, including anion exchange column 1, cation exchange column 2 and stirred tank 3, the upper portion of anion exchange column 1 is equipped with anion exchange liquid inlet 101, and the bottom is equipped with anion exchange liquid outlet 102, anion exchange liquid inlet 101 is connected through pipeline industrial grade polycarboxylic acid aqueous solution delivery pipeline and is connected in series valve, electronic flowmeter and transmission pump,

[0020] The upper portion of cation exchange column 2 is equipped with cation exchange liquid inlet 201, and the bottom is equipped with cation exchange liquid outlet 202, and cation exchange liquid inlet 201 is connected through pipeline anion exchange column's cation exchange liquid outlet 202 and is connected in series valve, electronic flowmeter and transmission pump,

[0021] The top of stirred tank 3 is equipped with stirring liquid inlet 301 and stirring resin inlet 302, and the bottom is equipped with stirring discharge port 303, and the outer wall is equipped with stirring constant-temperature heat exchanger 304, stirring liquid inlet 301 is connected through tee joint 4 cation exchange column 2 and electronic grade polycarboxylic acid transmission pipeline respectively, stirring resin inlet 302 is connected through pipeline resin weighing tank and is connected in series valve, stirring discharge port 303 is connected through pipeline electronic grade polycarboxylic acid transmission pipeline and is connected in series valve, electronic flowmeter and suction filter pump.

[0022] Anion exchange column 1 and cation exchange column 2 are both cylindrical, and the inner diameter of the cross section is 3-10 cm, and the length-diameter ratio is 20-30:1.

[0023] The left end of tee joint 4 is connected through pipeline cation exchange liquid outlet 202 and is connected in series valve, and the upper end is connected through pipeline stirring liquid inlet 301 and is connected in series valve, electronic flowmeter and transmission pump, and the right end is connected through pipeline electronic grade polycarboxylic acid transmission pipeline and is connected in series valve, electronic flowmeter and transmission pump.

[0024] Anion exchange column 1, cation exchange column 2 and stirred tank 3 can be parallelly connected according to actual needs, and N is greater than or equal to 2.

[0025] Specifically, the main equipment and raw material specifications in the device are as follows:

[0026] The inner diameter of the cross section of anion exchange column 1 and cation exchange column 2 is 5 cm, and the length is 1.2 m, and two of each are connected in parallel.

[0027] Stirred tank 3 is a 2000L porcelain shell kettle, and two are connected in parallel.

[0028] The anion exchange resin uses OH type anion exchange resin, the cation exchange resin uses hydrogen type cation exchange resin, and the anion exchange resin and the cation exchange resin are both spherical particles, and the diameter is about 1-2 mm.

[0029] The industrial polycarboxylic acid is self-produced by the company.

[0030] Preparation:

[0031] Fill the prepared anion exchange column 1 with OH type anion exchange resin, fill the prepared cation exchange resin with hydrogen type cation exchange resin, and reserve; dilute the industrial polycarboxylic acid aqueous solution to a mass fraction of 15% with pure water, and reserve.

[0032] Embodiment of production using the device

[0033] Step 1: open the corresponding valves, pump the polycarboxylic acid aqueous solution from the anion exchange inlet 101 into the anion exchange column 1 at a rate of 100 g / min to exchange and adsorb anions such as sulfate, after a period of time, start the liquid from the anion exchange outlet 102, and then enter the cation exchange column 2 through the cation exchange inlet 201 to exchange and adsorb metal ions, after a period of time, start the liquid from the cation exchange outlet 202, and the outflow is the qualified electronic grade polycarboxylic acid aqueous solution, which is pumped into the electronic grade polycarboxylic acid aqueous solution storage tank through the valve control of the three-way valve 4.

[0034] Step 2: continue to exchange for a period of time, the metal ion content of the polycarboxylic acid aqueous solution flowing out from the cation exchange outlet 202 increases, which no longer meets the electronic grade requirements, and the outflow at this time is pumped into the stirred tank 3 through the stirring inlet 301 through the valve control of the three-way valve 4, and after a certain mass of outflow is collected, the outflow is transferred into the parallel stirred tank 3 through valve control.

[0035] Step 3: add 1% hydrogen type cation exchange resin of the mass of the liquid in the tank to the stirred tank 3 through the stirring resin inlet 302, start stirring, control the temperature in the tank to be 20-40℃ through the stirring constant-temperature heat exchanger 304, stop stirring after 1 h, and the liquid in the tank is the qualified electronic grade polycarboxylic acid aqueous solution, which is pumped into the electronic grade polycarboxylic acid aqueous solution storage tank through the stirring outlet 303 by opening and closing the corresponding valves.

[0036] Step 4: when the exchange and adsorption efficiency of the ion exchange resin in the anion exchange column 1 or the cation exchange column 2 reaches 90%, use the parallel ion exchange column through valve control, and the original ion exchange column is disassembled and replaced to meet continuous production, the regenerated resin is reused, and the operation of the parallel stirred tank 3 is synchronized with step 3.

[0037] The above describes the preferred embodiment of the present application, and for ordinary skilled persons in the art, according to the teaching of the present application, the changes, modifications, replacements and variations of the embodiments without departing from the principles and spirits of the present application still fall within the protection scope of the present application.

Claims

1. A purification apparatus for an electronic grade polycarboxylic acid product, characterized by, It comprises an anion exchange column (1), a cation exchange column (2) and a stirring tank (3), the upper part of the anion exchange column (1) is provided with an anion exchange liquid inlet (101), the bottom is provided with an anion exchange liquid outlet (102), the anion exchange liquid inlet (101) is connected with an industrial polycarboxylic acid aqueous solution conveying pipeline through a pipeline and is connected with a valve, an electronic flowmeter and a transmission pump in series; The upper part of the cation exchange column (2) is provided with a cation exchange liquid inlet (201), the bottom is provided with a cation exchange liquid outlet (202), the cation exchange liquid inlet (201) is connected with the cation exchange liquid outlet (202) of the anion exchange column (1) through a pipeline and is connected with a valve, an electronic flowmeter and a transmission pump in series; The top of the stirring tank (3) is provided with a stirring liquid inlet (301) and a stirring resin inlet (302), the bottom is provided with a stirring discharge port (303), the outer wall is provided with a stirring constant-temperature heat exchanger (304), the stirring liquid inlet (301) is connected with the cation exchange column (2) and an electronic grade polycarboxylic acid conveying pipeline through a tee joint (4), the stirring resin inlet (302) is connected with a resin weighing tank through a pipeline and is connected with a valve in series, the stirring discharge port (303) is connected with an electronic grade polycarboxylic acid conveying pipeline through a pipeline and is connected with a valve, an electronic flowmeter and a suction filter pump in series.

2. A purification apparatus for electronic grade polycarboxylic acid product according to claim 1, characterized in that, The anion exchange column (1) and the cation exchange column (2) are both cylindrical, the cross-sectional inner diameter is 3-10 cm, and the length-diameter ratio is (20-30):

1.

3. A device for purifying an electronic grade polycarboxylic acid product according to claim 1, characterized in that, The left end of the tee joint (4) is connected with the cation exchange liquid outlet (202) through a pipeline and is connected with a valve in series; the upper end is connected with the stirring liquid inlet (301) through a pipeline and is connected with a valve, an electronic flowmeter and a transmission pump in series; the right end is connected with an electronic grade polycarboxylic acid conveying pipeline through a pipeline and is connected with a valve, an electronic flowmeter and a transmission pump in series.

4. A purification apparatus for electronic grade polycarboxylic acid product as claimed in claim 1, wherein, The anion exchange column (1), the cation exchange column (2) and the stirring tank (3) can be connected in parallel according to actual needs, N≥2.

5. A purification apparatus for electronic grade polycarboxylic acid product as claimed in claim 2, wherein, The cross-sectional inner diameter of the anion exchange column (1) and the cation exchange column (2) is 5 cm, and the length is 1.2 m, and two groups are connected in parallel.

6. A device for purifying an electronic grade polycarboxylic acid product according to claim 2, characterized in that, The stirring tank (3) is a 2000L enamel tank, and two are connected in parallel.

7. A device for purifying an electronic grade polycarboxylic acid product according to claim 2, characterized in that, The anion exchange resin uses OH type anion exchange resin, the cation exchange resin uses hydrogen type cation exchange resin, and the anion exchange resin and the cation exchange resin are both spherical particles with a diameter of about 1-2 mm.

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