CN107902632A - A kind of electronic-grade sulfuric acid heating unit and method - Google Patents

A kind of electronic-grade sulfuric acid heating unit and method Download PDF

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Publication number
CN107902632A
CN107902632A CN201711293206.8A CN201711293206A CN107902632A CN 107902632 A CN107902632 A CN 107902632A CN 201711293206 A CN201711293206 A CN 201711293206A CN 107902632 A CN107902632 A CN 107902632A
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CN
China
Prior art keywords
sulfuric acid
electronic
acidproof
housing
grade sulfuric
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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CN201711293206.8A
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Chinese (zh)
Inventor
王海
赵晓亚
程文海
曾朵清
李平
卢振成
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
ZHEJIANG KAISN FLUOROCHEMICAL CO Ltd
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ZHEJIANG KAISN FLUOROCHEMICAL CO Ltd
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Priority to CN201711293206.8A priority Critical patent/CN107902632A/en
Publication of CN107902632A publication Critical patent/CN107902632A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00Sulfur; Compounds thereof
    • C01B17/69Sulfur trioxide; Sulfuric acid
    • C01B17/90Separation; Purification

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The present invention provides a kind of electronic-grade sulfuric acid heating unit, including acidproof housing and at least one heater, heater is fixed on lower part in acidproof housing, and agitating device is provided with acidproof housing, the upper end of acidproof housing is provided with liquid-inlet, and acidproof housing bottom is provided with liquid outlet.The invention also discloses the method using device heating electronic-grade sulfuric acid.The configuration of the present invention is simple, easy to operate, the efficiency of heating surface is high, and after being heated by the device, the filter effect of electronic-grade sulfuric acid is greatly improved, and particle quality is greatly improved.

Description

A kind of electronic-grade sulfuric acid heating unit and method
Technical field
The present invention relates to electronic chemical product field, more particularly to a kind of electronic-grade sulfuric acid heating unit and method.
Background technology
At present, it is after the electronic-grade sulfuric acid solution that absorption has configured is cooled to room temperature in electronic-grade sulfuric acid production process Into pan tank, then from the circulating filtration of pan tank progress particle.As CN102530885B discloses a kind of high-purity sulphuric acid Industrialized preparing process, comprises the following steps:A, 40% nicotinic acid is evaporated into high-purity SO with nicotinic acid generator3Gas;B, AR is used Sulfuric acid absorption tower absorbs SO3;C, cooled down and shunted, the pipe between AR sulfuric acid absorption towers and AR sulfuric acid pump grooves by AR sulfuric acid pumps groove Desalted water or ultra-pure water are added on road, control sulfuric acid concentration gets to AR 98.5%, from the sour part of AR sulfuric acid pumps groove out The acid trap of sulfuric acid absorption tower absorbs SO as recycle acid3Flue gas, another part acid enter finished acid pump groove;D, finished acid pump groove In AR sulfuric acid coolers the acid of entrance is cooled down;E, finished product is become after being filtered by filter.
But viscosity is larger at normal temperatures for sulfuric acid solution, (physical filtering mistake during chemicals filter progress circulating filtration is utilized Journey), cause filter effect and filtration time to be all affected because viscosity is too big.In order to solve the problems, such as this, CN206064166U discloses a kind of filtration system for being used for MOS grades of electronics sulfuric acid production systems, including sulfuric acid filter and SO3 Pneumatic filter, SO3One layer of heating system has been wrapped up on pneumatic filter side wall.The patent heating system is substantially to solve SO3The problem of heating vaporization, because SO3Room temperature is solid, still no to solve the problems, such as that the big filtering of electronic-grade sulfuric acid viscosity is difficult.
On the other hand, although the boiling point of sulfuric acid and viscosity are higher, generally it is not easily decomposed, sulfuric acid is heated to meeting at 290 DEG C Start to decompose to give off sulfur trioxide, and the excessive moisture that can also volatilize of temperature, so electronic-grade sulfuric acid heating system must take into consideration Sulfate liquid local temperature cannot be made excessive, the prior art does not also propose solution for this technical problem.
The content of the invention
The present invention in view of the deficiencies of the prior art, there is provided it is a kind of it is simple in structure, easy to operate, the efficiency of heating surface is high Electronic-grade sulfuric acid heating unit and method.
In order to solve the above-mentioned technical problem, the present invention is achieved by the following technical solutions:A kind of electronic-grade sulfuric acid adds Thermal, including acidproof housing and at least one heater, the heater is fixed on lower part in the acidproof housing, described resistance to Agitating device is provided with sour housing, the upper end of the acidproof housing is provided with liquid-inlet, and the acidproof housing bottom is set There is liquid outlet.
Further:
The agitating device includes agitating shaft and the stirring slurry being arranged on the agitating shaft.
The heating tube material of the heater is preferably PTFE.
The acidproof housing includes shell and inner casing, and the enclosure material is preferably carbon steel, shell material in the acidproof housing It is of fine quality to elect PTFE as.
The stirring slurry radius is preferably 0.3~0.8 times of the agitating shaft and the heater distance.
The present invention also provides the method using above device heating electronic-grade sulfuric acid, comprise the following steps:
(1) electronic-grade sulfuric acid for absorbing and having configured is added into acidproof housing by liquid-inlet, starts heater and starts Electronic-grade sulfuric acid is heated;
(2) when electronic-grade sulfuric acid temperature rises to 20~30 DEG C, start agitating device and electronic-grade sulfuric acid is stirred;
(3) when electronic-grade sulfuric acid temperature reaches 45-65 DEG C, electronic-grade sulfuric acid is entered filtering by liquid outlet 5 is System.
98% electronic-grade sulfuric acid can raise the enhancing of its corrosivity with temperature, it is impossible to using traditional carbon steel material container, institute With all in the present invention and component of 98% electronic-grade sulfuric acid media contact all using PTFE.Other 98% electronic-grade sulfuric acid The resistance that viscosity size produces filter membrane has a significant impact, if electronic-grade sulfuric acid viscosity is excessive, can increase the dynamic of delivery pump Power consumes, and can reduce filter effect.And filter pressure is excessive, filtering bore dia has certain increase, causes bulky grain Possibly into the electronic-grade sulfuric acid liquid after filtering.
In order to reduce the viscosity of electronic-grade sulfuric acid liquid, the present invention is not polluting the electronic-grade sulfuric acid solution condition that has configured Under, 45-65 DEG C is brought up to using by the temperature of electronic-grade sulfuric acid liquid, such electronic-grade sulfuric acid liquid viscosity can decline to a great extent, Electronic-grade sulfuric acid liquid viscosity drops to 10cp or so from 20cp or so, so as to substantially improve filter effect, shortens filtering Time, and effectively prevent heating-up temperature it is excessive caused by electronic-grade sulfuric acid liquid decompose to give off sulfur trioxide and moisture evaporation is asked Topic.The heating-up temperature of another aspect electronic-grade sulfuric acid liquid is maintained at 45-65 DEG C, not only can greatly improve filter effect, and And it can prevent electronic-grade sulfuric acid fluid temperature is excessive to cause PTFE filter membrane varying apertures.
Electronic-grade sulfuric acid fluid temperature in order to prevent near heater is excessive, prevents sulfuric acid from decomposing, and the present invention exists An agitating device is provided with the sour housing of storage, by the agitation of agitating device, electronic-grade sulfuric acid liquid thermally equivalent can be made.
Compared with prior art, the present invention has the following advantages:
1st, simple in structure, easy to operate, electronic-grade sulfuric acid heating unit of the invention is simple in structure, enormously simplify operation Flow;
2nd, the efficiency of heating surface is high, during by the electronic-grade sulfuric acid heating devices heat electronic-grade sulfuric acid of the present invention, electron level sulphur Acid is heated evenly, it is therefore prevented that sulfuric acid is decomposed, and improves the efficiency of heating surface;
3rd, good product quality, after being heated by the device, the filter effect of electronic-grade sulfuric acid is greatly improved, contracting Short filtration time, reduces energy consumption;Following for particle is directly carried out with absorbing after the sulfuric acid solution configured is cooled to room temperature Ring filtering contrast, 0.04 μm of particle of electronic-grade sulfuric acid is dropped within 100Ea/ml from 2000~5000Ea/ml after filtering, circulation Filtration time saves 60~70%.
Brief description of the drawings
Fig. 1 is the structure diagram of the electronic-grade sulfuric acid heating unit of the present invention.
As shown in the figure, 1 is heater, 2 be acidproof housing, and 3 be agitating device, and 4 be liquid-inlet, and 5 be liquid outlet.
Embodiment
As shown in Figure 1, a kind of electronic-grade sulfuric acid heating unit, including acidproof housing 2 and at least one heater 1, heating Device 1 is fixed on lower part in acidproof housing 2, and agitating device 3 is provided with acidproof housing 2, and the upper end of the acidproof housing 2 is provided with Liquid-inlet 3, acidproof 2 bottom of housing are provided with liquid outlet 5.Agitating device 3 includes agitating shaft and is arranged on agitating shaft Stirring slurry.
Using the device heating electronic-grade sulfuric acid flow be:Absorption is added by liquid-inlet 4 into acidproof housing 2 to match somebody with somebody The electronic-grade sulfuric acid put, starts heater 1 and starts to heat electronic-grade sulfuric acid;Electron level sulphur in acidproof housing 2 When sour temperature rises to 20~30 DEG C, start agitating device 3 and electronic-grade sulfuric acid is stirred, make electronic-grade sulfuric acid thermally equivalent; When electronic-grade sulfuric acid temperature reaches 45-65 DEG C, electronic-grade sulfuric acid is entered into filtration system by liquid outlet 5.
The present invention is described in more detail by the following examples, but protection scope of the present invention is not limited to these Embodiment.
Embodiment 1
A kind of electronic-grade sulfuric acid heating unit, including acidproof housing 2 and a heater 1 (heating tube material is PTFE), Heater 1 is fixed on lower part in acidproof housing 2, and agitating device 3 is provided with acidproof housing 2, and the upper end of acidproof housing 2 is provided with Liquid-inlet 3, acidproof 2 bottom of housing are provided with liquid outlet 5.Agitating device 3 includes agitating shaft and is arranged on agitating shaft Stirring slurry 0.3 times of agitating shaft and heater distance (stirring slurry radius for), acidproof housing 2 include shell (material is carbon steel) and Inner casing (material PTFE).
Using the device heating electronic-grade sulfuric acid flow be:Absorption is added by liquid-inlet 4 into acidproof housing 2 to match somebody with somebody The electronic-grade sulfuric acid put, starts heater 1 and starts to heat electronic-grade sulfuric acid;Electron level sulphur in acidproof housing 2 When sour temperature rises to 20 DEG C, start agitating device 3 and electronic-grade sulfuric acid is stirred, make electronic-grade sulfuric acid thermally equivalent;Work as electricity When sub- level sulfuric acid temperature reaches 45 DEG C, electronic-grade sulfuric acid is entered into filtration system by liquid outlet 5.
Refiltered after heating electronic-grade sulfuric acid using the device, 0.04 μm of particle drops to 40Ea/ from 2000Ea/ml ml;Circulating filtration contrast with absorbing directly progress particle after the sulfuric acid solution that configure is cooled to room temperature, during circulating filtration Between save 70%.
Embodiment 2
A kind of electronic-grade sulfuric acid heating unit, including acidproof housing 2 and two heaters 1 (heating tube material is PTFE), Heater 1 is fixed on lower part in acidproof housing 2, and agitating device 3 is provided with acidproof housing 2, and the upper end of acidproof housing 2 is provided with Liquid-inlet 3, acidproof 2 bottom of housing are provided with liquid outlet 5.Agitating device 3 includes agitating shaft and is arranged on agitating shaft Stirring slurry 0.5 times of agitating shaft and heater distance (stirring slurry radius for), acidproof housing 2 include shell (material is carbon steel) and Inner casing (material PTFE).
Using the device heating electronic-grade sulfuric acid flow be:Absorption is added by liquid-inlet 4 into acidproof housing 2 to match somebody with somebody The electronic-grade sulfuric acid put, starts heater 1 and starts to heat electronic-grade sulfuric acid;Electron level sulphur in acidproof housing 2 When sour temperature rises to 25 DEG C, start agitating device 3 and electronic-grade sulfuric acid is stirred, make electronic-grade sulfuric acid thermally equivalent;Work as electricity When sub- level sulfuric acid temperature reaches 50 DEG C, electronic-grade sulfuric acid is entered into filtration system by liquid outlet 5.
Refiltered after heating electronic-grade sulfuric acid using the device, 0.04 μm of particle drops to 60Ea/ml from 3000Ea/ml It is interior;Circulating filtration contrast with absorbing directly progress particle after the sulfuric acid solution that configure is cooled to room temperature, during circulating filtration Between save 65%.
Embodiment 3
A kind of electronic-grade sulfuric acid heating unit, including acidproof housing 2 and three heaters 1 (heating tube material is PTFE), Heater 1 is fixed on lower part in acidproof housing 2, and agitating device 3 is provided with acidproof housing 2, and the upper end of acidproof housing 2 is provided with Liquid-inlet 3, acidproof 2 bottom of housing are provided with liquid outlet 5.Agitating device 3 includes agitating shaft and is arranged on agitating shaft Stirring slurry 0.7 times of agitating shaft and heater distance (stirring slurry radius for), acidproof housing 2 include shell (material is carbon steel) and Inner casing (material PTFE).
Using the device heating electronic-grade sulfuric acid flow be:Absorption is added by liquid-inlet 4 into acidproof housing 2 to match somebody with somebody The electronic-grade sulfuric acid put, starts heater 1 and starts to heat electronic-grade sulfuric acid;Electron level sulphur in acidproof housing 2 When sour temperature rises to 28 DEG C, start agitating device 3 and electronic-grade sulfuric acid is stirred, make electronic-grade sulfuric acid thermally equivalent;Work as electricity When sub- level sulfuric acid temperature reaches 55 DEG C, electronic-grade sulfuric acid is entered into filtration system by liquid outlet 5.
Refiltered after heating electronic-grade sulfuric acid using the device, 0.04 μm of particle drops to 80Ea/m from 4000Ea/ml; Circulating filtration contrast with absorbing directly progress particle after the sulfuric acid solution that configure is cooled to room temperature, segmentum intercalaris during circulating filtration Save 63%.
Embodiment 4
A kind of electronic-grade sulfuric acid heating unit, including acidproof housing 2 and four heaters 1 (heating tube material is PTFE), Heater 1 is fixed on lower part in acidproof housing 2, and agitating device 3 is provided with acidproof housing 2, and the upper end of acidproof housing 2 is provided with Liquid-inlet 3, acidproof 2 bottom of housing are provided with liquid outlet 5.Agitating device 3 includes agitating shaft and is arranged on agitating shaft Stirring slurry 0.8 times of agitating shaft and heater distance (stirring slurry radius for), acidproof housing 2 include shell (material is carbon steel) and Inner casing (material PTFE).
Using the device heating electronic-grade sulfuric acid flow be:Absorption is added by liquid-inlet 4 into acidproof housing 2 to match somebody with somebody The electronic-grade sulfuric acid put, starts heater 1 and starts to heat electronic-grade sulfuric acid;Electron level sulphur in acidproof housing 2 When sour temperature rises to 30 DEG C, start agitating device 3 and electronic-grade sulfuric acid is stirred, make electronic-grade sulfuric acid thermally equivalent;Work as electricity When sub- level sulfuric acid temperature reaches 65 DEG C, electronic-grade sulfuric acid is entered into filtration system by liquid outlet 5.
Refiltered after heating electronic-grade sulfuric acid using the device, 0.04 μm of particle drops to 100Ea/ from 5000Ea/ml ml;Circulating filtration contrast with absorbing directly progress particle after the sulfuric acid solution that configure is cooled to room temperature, during circulating filtration Between save 60%.

Claims (6)

1. a kind of electronic-grade sulfuric acid heating unit, including acidproof housing and at least one heater, it is characterised in that the heating Device is fixed on lower part in the acidproof housing, and agitating device is provided with the acidproof housing, and the upper end of the acidproof housing is set Liquid-inlet is equipped with, the acidproof housing bottom is provided with liquid outlet.
2. electronic-grade sulfuric acid heating unit according to claim 1, it is characterised in that the agitating device includes agitating shaft With the stirring slurry being arranged on the agitating shaft.
3. electronic-grade sulfuric acid heating unit according to claim 1, it is characterised in that the heating tube material of the heater For PTFE.
4. electronic-grade sulfuric acid heating unit according to claim 1, it is characterised in that the acidproof housing include shell and Inner casing, the enclosure material are carbon steel, and the acidproof housing inner casing material is PTFE.
5. electronic-grade sulfuric acid heating unit according to claim 2, it is characterised in that the stirring slurry radius stirs to be described Mix axis and the heater distance 0.3~0.8 times.
6. the method for the device heating electronic-grade sulfuric acid of usage right requirement 1, it is characterised in that comprise the following steps:
(1) electronic-grade sulfuric acid for absorbing and having configured is added into acidproof housing by liquid-inlet, starts heater and starts to electricity Sub- level sulfuric acid is heated;
(2) when electronic-grade sulfuric acid temperature rises to 20~30 DEG C, start agitating device and electronic-grade sulfuric acid is stirred;
(3) when electronic-grade sulfuric acid temperature reaches 45-65 DEG C, electronic-grade sulfuric acid is entered into filtration system by liquid outlet.
CN201711293206.8A 2017-12-08 2017-12-08 A kind of electronic-grade sulfuric acid heating unit and method Pending CN107902632A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201711293206.8A CN107902632A (en) 2017-12-08 2017-12-08 A kind of electronic-grade sulfuric acid heating unit and method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711293206.8A CN107902632A (en) 2017-12-08 2017-12-08 A kind of electronic-grade sulfuric acid heating unit and method

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN203342816U (en) * 2013-06-08 2013-12-18 天津市亨益晟泰筑路材料科技有限公司 Reaction kettle for producing self-emulsifying water-borne epoxy resin
CN204454587U (en) * 2015-03-18 2015-07-08 苏州晶瑞化学有限公司 A kind of ultra-clean and high-purity sulphuric acid High-efficient Production device
CN207792695U (en) * 2017-12-08 2018-08-31 浙江凯圣氟化学有限公司 A kind of electronic-grade sulfuric acid heating device

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN203342816U (en) * 2013-06-08 2013-12-18 天津市亨益晟泰筑路材料科技有限公司 Reaction kettle for producing self-emulsifying water-borne epoxy resin
CN204454587U (en) * 2015-03-18 2015-07-08 苏州晶瑞化学有限公司 A kind of ultra-clean and high-purity sulphuric acid High-efficient Production device
CN207792695U (en) * 2017-12-08 2018-08-31 浙江凯圣氟化学有限公司 A kind of electronic-grade sulfuric acid heating device

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