A kind of production equipment of high-purity hydrogen peroxide
Technical field
The utility model is related to a kind of production equipment of high-purity hydrogen peroxide, especially semiconductor and ICs with high-purity
The production equipment of hydrogen peroxide.
Background technology
High-purity hydrogen peroxide plays an important role in electronic manufacturing field, is widely used in the cleaning of semiconductor and IC
Corrosion etc., higher and higher to the quality requirement of high-purity hydrogen peroxide with the development of electronics industry, demand is also increasing.I
The existing industrial grade hydrogen peroxide of state mostly uses greatly anthraquinone production, and the advantages of this method is that technology maturation is at low cost, but product
In contain a large amount of organic and inorganic impurity.It is industrial usually using distillation, reverse osmosis, ion exchange to eliminate these impurity
The methods of, but production cost is high, low production efficiency, poor product quality.
Currently, there are two ways to industrialization purifying hydrogen peroxide:First, adding cation and anion exchange using organic carbon adsorption
Method, such as CN1285311A, it is that raw material hydrogen peroxide is inputted the absorption that adsorption resin column carries out organic carbon by pump, then will
The hydrogen peroxide input anion-cation exchange resin column for removing organic carbon carries out ion exchange, then by the peroxide Jing Guo ion exchange
Change hydrogen input filter to remove granule foreign, to obtain ultrapure hydrogen peroxide product.Second is that being handed over using single zwitterion
It changes and adds cation and anion exchange method, such as CN1439600A.It is by industrial hydrogen peroxide solution continue to flow through anion exchange resin,
Anion exchange resin and negative and positive mixture iron exchange resin carry out ion exchange, and high-purity hydrogen peroxide product is made.The two is equal
There are raw material hydrogen peroxide utilization rate is low, only 85%, the defects of production cost is high, inferior separating effect, purity does not reach requirement.
Product purity does not meet semiconductor equipment and material structure (SEMI-C8) standard, i.e. metal ion content hour 1PPb, has
Machine carbon content is less than 20PPm.Semiconductor equipment and material structure SEMIC19-90 and SEMIC7 can only be met
5-93 standards.
CN1184138C discloses a kind of manufacturing process and equipment of ultrapure hydrogen peroxide, but its production cost compared with
Height, separating effect are also to be hoisted.
Invention content
Technical problem to be solved in the utility model is to provide a kind of high-purity hydrogen peroxide for the above-mentioned prior art
Production equipment, solves that traditional hydrogen peroxide method of purification production cost is high, efficiency is low, ropy disadvantage.
The technical scheme in the invention for solving the above technical problem is:A kind of production equipment of high-purity hydrogen peroxide,
It is provided with high-order storage tank, adsorption resin column, ion exchange resin column, intermediate storage tank, nanofiltration membrane component, finished product storage from top to bottom
Tank;High-order reservoir outlet is connect by pipeline with adsorption resin column upper inlet, and valve K1 is equipped on pipeline;Adsorb resin
Outlet is connect by pipeline with ion exchange column upper inlet and is equipped with valve K2 under column;Outlet and intermediate storage tank under ion exchange column
Entrance connects and is equipped with valve K3;Intermediate storage tank is connected with vacuum pump and blow valve K4;Intermediate storage tank outlet is by pipeline in
Hollow fiber nanofiltration membrane component entrance is connected, and pipeline is equipped with valve K5 and booster pump;Under hollow fiber nanofiltration membrane component outlet with
Finished product storage tank entrance is connected, and valve K6 is equipped in connecting pipe.
Further, a diameter of 200mm of adsorption resin column is highly 1000-1200mm;The absorption resin of filling is benzene second
The mixture of alkene or divinylbenzene or styrene and divinylbenzene.Preferably macropore made of styrene, divinylbenzene copolymerization is inhaled
Attached resin.
Further, a diameter of 200mm of ion exchange resin column is highly 1000-1400mm;Ion exchange resin column
The filler material at bottom one third position is the mixture of anion-cation exchange resin equal proportion, the filling of intermediate one third
Material be cation exchange resin, above one third filler material be anion exchange resin.
Further, hollow fiber nanofiltration membrane component is external-compression type component.
The production technology of the high-purity hydrogen peroxide includes the following steps:
(1)Impurity removes the stage:It adsorbs resin and removes organic carbon contaminants and ion exchange removing unit second cation impurity;
Direct storage exists in high-order storage tank after primary industry hydrogen peroxide incoming inspection qualification, K4 and K5 is closed when purification produces, successively
Vacuum pump, K3, K2, K1 are opened, allows industrial hydrogen peroxide to pass sequentially through adsorption resin column, intermediate storage is stored in after ion exchange column
Tank closes K1, K2, K3 and vacuum pump successively after the completion;
(2)The nanofiltration membrane stage opens K4, K5, K6 booster pump successively, makes the hydrogen peroxide pressurization in intermediate storage tank logical
Hollow fiber nanofiltration membrane component is crossed, residual impurity ion is removed, obtains high-purity hydrogen peroxide.
Further, the running temperature in impurity removal stage is 10-30 DEG C, and operating pressure is to vacuumize negative pressure, absolute pressure
Power is controlled in 40-50kp;The running temperature in nanofiltration membrane stage is 10-30 DEG C, and operating pressure is pressurization, and absolute pressure is
500-600kp。
The utility model technology is divided to two sections of progress, first segment to be that absorption resin adsorption organic carbon and ion exchange remove
Part zwitterion impurity.Direct storage exists in high-order storage tank after primary industry hydrogen peroxide incoming inspection qualification, purification production
When close K4 and K5, open vacuum pump, K3, K2, K1 successively, industrial hydrogen peroxide allowed to pass sequentially through adsorption resin column, ion is handed over
It is stored in intermediate storage tank after changing column, closes K1, K2, K3 and vacuum pump successively after the completion.Above-mentioned adsorption resin column is a diameter of
200mm is highly 1000-1200mm, and absorption resin used is styrene or divinylbenzene or styrene and divinylbenzene
Mixture.The above-mentioned a diameter of 200mm of ion exchange resin column, is highly 1000-1400mm, and filler is anion exchange
Resin and cation exchange resin, and the mixture that bottom one third is anion-cation exchange resin equal proportion, centre three
/ mono- be cation exchange resin, above one third be anion exchange resin.This section of production technology pressure control is in 40-
50kp, temperature are controlled at 10-30 degrees Celsius.Second segment is the nanofiltration membrane stage, removes residual impurity ion.It opens successively
K4, K5, K6 booster pump allow the hydrogen peroxide in intermediate storage tank to be forced through hollow fiber nanofiltration membrane component, remove foreign ion,
Obtain high-purity hydrogen peroxide.Above-mentioned doughnut nanofiltration membrane component is external-compression type component, this section of production technology pressure control exists
500-600kp, temperature are controlled at 10-30 DEG C.
Compared with prior art, the utility model advantageous effects:
(1)Each device is arranged by high order from top to bottom for the utility model can make full use of potential energy, and at
It is provided with intermediate storage tank between product storage tank and high-order storage tank, makes the utility model only two pumps need to be arranged to can be driven, drops significantly
Low production cost;
(2)The ion exchange resin column difference from prior art of the utility model is subsection filling different proportion
Anion-cation exchange resin fills anion exchange resin in the top, and interlude is cation exchange resin, and bottom is etc.
The anion-cation exchange resin of ratio, this filling mode can carry out grading absorption, and subsequent recovery is facilitated to reuse,
To substantially reduce cost;
(3)The utility model is designed by overall flow, greatly reduces the required pressure of production technology, low to realize
Cost produces, and by the setting of segmented ion exchange resin column and hollow fiber nanofiltration membrane, improves the absorption to impurity
Ability keeps the product quality of preparation more preferable.
Description of the drawings
Fig. 1 is the production technological process of the utility model.
Wherein:High-order storage tank 1, adsorption resin column 2, ion exchange resin column 3, intermediate storage tank 4, nanofiltration membrane component 5, finished product
Storage tank 6.
Specific implementation mode
The utility model is described in further detail below in conjunction with attached drawing embodiment.
The utility model is illustrated with reference to embodiment.
A kind of production equipment of high-purity hydrogen peroxide, is provided with high-order storage tank 1, adsorption resin column 2 from top to bottom, and ion is handed over
Change resin column 3, intermediate storage tank 4, nanofiltration membrane component 5 and finished product storage tank 6;1 discharge port of high-order storage tank passes through pipeline and absorption resin
2 upper inlet of column connects, and valve K1 is equipped on pipeline;2 times outlets of adsorption resin column and 3 upper inlet of ion exchange resin column are logical
Piping connects and is equipped with valve K2;3 times outlets of ion exchange resin column connect with 4 entrance of intermediate storage tank and are equipped with valve K3;
Intermediate storage tank 4 is connected with vacuum pump and blow valve K4;The outlet of intermediate storage tank 4 is entered by pipeline with hollow fiber nanofiltration membrane component 5
Mouth is connected, and pipeline is equipped with valve K5 and booster pump;The 5 times outlets of hollow fiber nanofiltration membrane component are connected with 6 entrance of finished product storage tank,
And valve K6 is equipped in connecting pipe.
Embodiment 1
First segment is absorption resin adsorption and ion exchange.It is directly stored after primary industry hydrogen peroxide incoming inspection qualification
In high-order storage tank, purification production when close K4 and K5, successively open vacuum pump, K3, K2, K1, allow industrial hydrogen peroxide successively
By adsorption resin column, it is stored in intermediate storage tank after ion exchange column, closes K1, K2, K3 and vacuum pump successively after the completion.It is above-mentioned
The a diameter of 200mm of adsorption resin column is highly 1000mm, and absorption resin used is styrene.Above-mentioned ion exchange resin column
A diameter of 200mm is highly 1000mm, and filler is anion exchange resin and cation exchange resin, and bottom
One third be anion-cation exchange resin equal proportion mixture, intermediate one third be cation exchange resin, above three
/ mono- is anion exchange resin.In 40kp, temperature is controlled at 10 DEG C for this section of production technology pressure control.
Second segment is the nanofiltration membrane stage, opens K4, K5, K6 booster pump successively, allows hydrogen peroxide in intermediate storage tank
It is forced through hollow fiber nanofiltration membrane component, foreign ion is removed, obtains high-purity hydrogen peroxide.Above-mentioned hollow fiber nanofiltration membrane group
Part is external-compression type component, and in 500kp, temperature is controlled at 10 DEG C for this section of production technology pressure control.
Embodiment 2
First segment is absorption resin adsorption and ion exchange.It is directly stored after primary industry hydrogen peroxide incoming inspection qualification
In high-order storage tank, purification production when close K4 and K5, successively open vacuum pump, K3, K2, K1, allow industrial hydrogen peroxide successively
By adsorption resin column, it is stored in intermediate storage tank after ion exchange column, closes K1, K2, K3 and vacuum pump successively after the completion.It is above-mentioned
The a diameter of 200mm of adsorption resin column is highly 1100mm, and absorption resin used is divinylbenzene.Above-mentioned ion exchange resin
Column diameter is 200mm, is highly 1200mm, and filler is anion exchange resin and cation exchange resin, and most lower
Face one third is the mixture of anion-cation exchange resin equal proportion, and intermediate one third is cation exchange resin, above
One third is anion exchange resin.In 45kp, temperature is controlled at 20 DEG C for this section of production technology pressure control.
Second segment is the nanofiltration membrane stage, opens K4, K5, K6 booster pump successively, allows hydrogen peroxide in intermediate storage tank
It is forced through hollow fiber nanofiltration membrane component, foreign ion is removed, obtains high-purity hydrogen peroxide.Above-mentioned hollow fiber nanofiltration membrane group
Part is external-compression type component, and in 550kp, temperature is controlled at 20 DEG C for this section of production technology pressure control.
Embodiment 3
First segment is absorption resin adsorption and ion exchange.It is directly stored after primary industry hydrogen peroxide incoming inspection qualification
In high-order storage tank, purification production when close K4 and K5, successively open vacuum pump, K3, K2, K1, allow industrial hydrogen peroxide successively
By adsorption resin column, it is stored in intermediate storage tank after ion exchange column, closes K1, K2, K3 and vacuum pump successively after the completion.It is above-mentioned
The a diameter of 200mm of adsorption resin column is highly 1200mm, and absorption resin used is the mixture of styrene and divinylbenzene.
The above-mentioned a diameter of 200mm of ion exchange resin column, is highly 1400mm, and filler is anion exchange resin and cation
Exchanger resin, and the mixture that bottom one third is anion-cation exchange resin equal proportion, intermediate one third be sun from
Sub-exchange resin, above one third be anion exchange resin.This section of production technology pressure control exists in 50kp, temperature control
30℃。
Second segment is the nanofiltration membrane stage, opens K4, K5, K6 booster pump successively, allows hydrogen peroxide in intermediate storage tank
It is forced through hollow fiber nanofiltration membrane component, foreign ion is removed, obtains high-purity hydrogen peroxide.Above-mentioned hollow fiber nanofiltration membrane group
Part is external-compression type component, and in 600kp, temperature is controlled at 30 DEG C for this section of production technology pressure control.
Comparative example 1
It is same as Example 3, in addition to all anion-cation exchange resin equal proportions of ion exchange resin column filler
Mixture.
Comparative example 2
It is produced according to the preparation process of the embodiment 1 of CN1184138C.
Test result is as follows shown in table:
It analyzes in above table in raw material and each embodiment known to the content of impurity:The utility model can be removed effectively
Organic carbon in hydrogen oxide and zwitterion impurity, and cost is lower, it is more efficient.In addition to the implementation, this practicality is new
Type further includes having other embodiment, and all technical solutions formed using equivalent transformation or equivalent replacement mode should all be fallen into
Within the protection domain of the utility model claims.