CN2663972Y - Near critical subaqueous solubility measuring apparatus - Google Patents

Near critical subaqueous solubility measuring apparatus Download PDF

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Publication number
CN2663972Y
CN2663972Y CN 200320122940 CN200320122940U CN2663972Y CN 2663972 Y CN2663972 Y CN 2663972Y CN 200320122940 CN200320122940 CN 200320122940 CN 200320122940 U CN200320122940 U CN 200320122940U CN 2663972 Y CN2663972 Y CN 2663972Y
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China
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valve
successively
critical water
sample
sampling
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Expired - Fee Related
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CN 200320122940
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Chinese (zh)
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吕秀阳
何龙
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The utility model discloses a near critical subaqueous solubility measuring apparatus, which is provided with an inlet system, a pressure compensation system, an equilibrium still, a temperature control system and a sampling system in turn, wherein, the inlet system is provided with a high pressure metering pump, a first valve, a second valve and a nitrogen steel cylinder in turn; the pressure compensation system is provided with a third valve, a fourth valve, a bugger tank, a fifth valve and a pressure gauge in turn; the equilibrium still is provided with a still body, a stirrer, a safety valve, a pressure gauge, an atmos valve and a liquid discharge valve; the temperature control system is provided with a heat preservation jacket and a temperature controller in turn; in addition, the pressure compensation system and the equilibrium still are connected through a sixth valve. The utility model has the advantages that: it can complete fast and accurate systematic measurement of organics/inorganics solubility in NCW; meanwhile, pressure change is small during sampling process, thereby being capable of ensuring representativeness of sample; moreover, with ideal versatility, the apparatus can measure solubility in near critical water and also can be used in research of stability and reaction kinetics in near critical water.

Description

Solubility test device in the near-critical water
Technical field
The utility model relates to the mensuration of solubility test device, especially organism solubleness in near-critical water in a kind of near-critical water.
Background technology
(near-critical water NCW), is meant the compressed liquid water of temperature between 200 ℃~350 ℃ to near-critical water.Good owing to mass-transfer performance, as self to have the function of acid catalysis and base catalysis and have energy while dissolved organic matter and inorganics characteristic, therefore its organic solvent that can substitute murder by poisoning carries out chemical reaction, even remove the adding of acid base catalysator from, make organic chemical reactions in NCW, the detachment process among the NCW, the renewable resources technology among the NCW etc. become one of focus in recent years.And, a natural abundance high important directions becoming Green Chemistry chemical industry development nontoxic, cheap with it.
Material solubleness in NCW is green chemical process necessary base data among the research and development NCW, have only reactant, intermediate and the final product dissolving situation in NCW that fullys understand a chemical reaction process, could grasp, control the carrying out of this course of reaction.But because the chemical process applied basic research also is in state at the early-stage among the NCW, the High Temperature High Pressure operating difficulties is very high to equipment requirements in addition, and basic data relevant among the NCW is lacked very much, has hindered the research and the application process of green chemical process among the NCW.
The solubility test method has three kinds of cloud point method, dynamic method and static methods etc. among the NCW.Because the cloud point method is to the equipment requirements height, dynamic method cannot say for sure that card reaches balance, so static method is the High Temperature High Pressure method commonly used in the research that balances each other.When static method is measured among the NCW solubleness, how to keep temperature, pressure condition in the equilibrium still constant, how under high pressure the sample in the equilibrium still to be taken out, and the sample that takes out is representative, and not change in sampling process be the gordian technique of measuring and form.At present, also there is not ripe perfect proving installation that solubleness among the NCW is carried out system measurement both at home and abroad.
Summary of the invention
The purpose of this utility model provides solubility test device in a kind of near-critical water.
It has sampling system successively, pressure compensating system, equilibrium still, temperature control system and sampling system, sampling system has high-pressure metering pump successively, first valve, second valve, the nitrogen steel cylinder, pressure compensating system has the 3rd valve successively, the 4th valve, surge tank, the 5th valve, tensimeter, equilibrium still has kettle, stirrer, safety valve, tensimeter, atmospheric valve, tapping valve, temperature control system has muff successively, temperature controller, on sampling system has, in, following three level sampling pipeline, the upper strata pipeline has first sample valve successively, second sample valve, quantity tube, the 3rd sample valve, relief tube, middle tube has the 4th sample valve successively, the 5th sample valve, quantity tube, the 6th sample valve, relief tube, lower floor's pipeline has the 7th sample valve successively, the 8th sample valve, quantity tube, the 9th sample valve, relief tube.Join with the 6th valve between pressure compensating system and equilibrium still.
Advantage of the present utility model: can be quick, accurately the organism among the NCW/inorganics solubleness is carried out system measurement, adopt surge tank to carry out ftercompction, sampling process pressure changes little; Adopt the sampling of semi-fluid dynamic formula quantity tube, can guarantee the representativeness of sample; Adopt PID to regulate temperature-controlled precision height (± 1 ℃); Kettle adopts titanium alloy TC 4, and is corrosion-resistant; The versatility of device is good, except measuring the solubleness in the near-critical water, also can be used for stability study, reaction kinetics research in the near-critical water.
Description of drawings
Fig. 1 is a solubility test apparatus structure synoptic diagram in the near-critical water;
Fig. 2 is the utility model sampling system structural representation.
Embodiment
As shown in Figure 1, the solubility test device has sampling system successively in the near-critical water, pressure compensating system, equilibrium still, temperature control system and sampling system 6, sampling system has high-pressure metering pump 1 successively, the first valve V1, the second valve V2, nitrogen steel cylinder 2, pressure compensating system has the 3rd valve V3 successively, the 4th valve V4, surge tank 3, the 5th valve V5, tensimeter P1, equilibrium still has kettle 8, stirrer 5, safety valve 4, tensimeter P2, atmospheric valve V7, tapping valve V8, temperature control system has muff 9 successively, temperature controller 10 joins with the 6th valve V6 between pressure compensating system and equilibrium still.
Sampling system 6 has the upper, middle and lower-ranking sampling line, the upper strata pipeline has the first sample valve S1, the second sample valve S2, quantity tube 7, the 3rd sample valve S3, relief tube 11 successively, middle tube has the 4th sample valve S4, the 5th sample valve S5, quantity tube 7, the 6th sample valve S6, relief tube 11 successively, and lower floor's pipeline has the 7th sample valve S7, the 8th sample valve S8, quantity tube 7, the 9th sample valve S9, relief tube 11 successively.
The volume of equilibrium still is 0.5L, and the volume of surge tank is 1L.Because near-critical water and test substance have certain corrosivity, kettle, temperature tube, shaft and slurry etc. adopt titanium alloy TC 4; Other parameter: 50~1000 rev/mins of working speeds, tensimeter (0~40MPa, 0.4 grade).
Pressure compensated principle is to charge into high pressure N before the experiment beginning in surge tank 2, by squeezing into pressure that water makes surge tank to the bottom of surge tank a little more than the pressure in the equilibrium still, the pressure loss that causes to equilibrium still compensation sampling of Open valve V6 as required.
As shown in Figure 2, S1 in the sampling system~S9 sample cock is high pressure valve (15-11AF1), adopts three sampling lines to get the sample of upper, middle and lower diverse location in the equilibrium still respectively.With article one stopple coupon is example, the pipe behind the valve S3 be relief tube (1/16 " OD * 0.006 " ID, SUS316), length is 60cm; The pipe of S3 front adopts 1/16 " OD * 0.030 " ID (SUS316); Be the sampling quantity tube between S2~S3,

Claims (6)

1. solubility test device in the near-critical water, it is characterized in that: it has sampling system successively, pressure compensating system, equilibrium still, temperature control system and sampling system (6), sampling system has high-pressure metering pump (1) successively, first valve (V1), second valve (V2), nitrogen steel cylinder (2), pressure compensating system has the 3rd valve (V3) successively, the 4th valve (V4), surge tank (3), the 5th valve (V5), tensimeter (P1), equilibrium still has kettle (8), stirrer (5), safety valve (4), tensimeter (P2), atmospheric valve (V7), tapping valve (V8), temperature control system has muff (9) successively, temperature controller (10) joins with the 6th valve (V6) between pressure compensating system and equilibrium still.
2. solubility test device in a kind of near-critical water according to claim 1, on it is characterized in that said sampling system (6) has, in, following three level sampling pipeline, the upper strata pipeline has first sample valve (S1) successively, second sample valve (S2), quantity tube (7), the 3rd sample valve (S3), relief tube (11), middle tube has the 4th sample valve (S4) successively, the 5th sample valve (S5), quantity tube (7), the 6th sample valve (S6), relief tube (11), lower floor's pipeline have the 7th sample valve (S7) successively, the 8th sample valve (S8), quantity tube (7), the 9th sample valve (S9), relief tube (11).
3. solubility test device in a kind of near-critical water according to claim 1 is characterized in that said equilibrium still adopts titanium alloy TC 4.
4. solubility test device in a kind of near-critical water according to claim 1 is characterized in that said temperature control system adopts PID to regulate.
5. solubility test device in a kind of near-critical water according to claim 1 is characterized in that said pressure compensating system adopts surge tank.
6. solubility test device in a kind of near-critical water according to claim 1 is characterized in that said sampling system adopts the sampling of semi-fluid dynamic formula quantity tube.
CN 200320122940 2003-12-26 2003-12-26 Near critical subaqueous solubility measuring apparatus Expired - Fee Related CN2663972Y (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 200320122940 CN2663972Y (en) 2003-12-26 2003-12-26 Near critical subaqueous solubility measuring apparatus

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Application Number Priority Date Filing Date Title
CN 200320122940 CN2663972Y (en) 2003-12-26 2003-12-26 Near critical subaqueous solubility measuring apparatus

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CN2663972Y true CN2663972Y (en) 2004-12-15

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102393344A (en) * 2011-10-17 2012-03-28 中国石油化工股份有限公司 Device for measuring solubility of gas in liquid with higher boiling point and method
CN103048165A (en) * 2011-10-15 2013-04-17 四川汇利实业有限公司 Sampling device for testing dissolubility by adopting automatic control process
CN105489094A (en) * 2016-01-07 2016-04-13 清华大学 Subcritical, supercritical pressure, temperature and phase state teaching experiment bench
CN105987862A (en) * 2015-01-28 2016-10-05 珠海格力节能环保制冷技术研究中心有限公司 Test apparatus and test method of dissolubility and viscosity
CN106525643A (en) * 2017-01-17 2017-03-22 中国石油大学(北京) Method for determining solubility of methane in petroleum
CN111624235A (en) * 2020-05-30 2020-09-04 西安交通大学 Flow type high-temperature high-pressure solubility online measuring device and measuring method thereof

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103048165A (en) * 2011-10-15 2013-04-17 四川汇利实业有限公司 Sampling device for testing dissolubility by adopting automatic control process
CN102393344A (en) * 2011-10-17 2012-03-28 中国石油化工股份有限公司 Device for measuring solubility of gas in liquid with higher boiling point and method
CN105987862A (en) * 2015-01-28 2016-10-05 珠海格力节能环保制冷技术研究中心有限公司 Test apparatus and test method of dissolubility and viscosity
CN105987862B (en) * 2015-01-28 2019-03-19 珠海格力节能环保制冷技术研究中心有限公司 The test device and method of solubility and viscosity
CN105489094A (en) * 2016-01-07 2016-04-13 清华大学 Subcritical, supercritical pressure, temperature and phase state teaching experiment bench
CN105489094B (en) * 2016-01-07 2018-01-05 清华大学 A kind of subcritical supercritical pressure, temperature and phase teaching experimental base
CN106525643A (en) * 2017-01-17 2017-03-22 中国石油大学(北京) Method for determining solubility of methane in petroleum
CN111624235A (en) * 2020-05-30 2020-09-04 西安交通大学 Flow type high-temperature high-pressure solubility online measuring device and measuring method thereof

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