CN102866214B - Method for detecting content of triethylamine in gas-phase condensed recovery liquid obtained from SAPO34 preparation - Google Patents
Method for detecting content of triethylamine in gas-phase condensed recovery liquid obtained from SAPO34 preparation Download PDFInfo
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- CN102866214B CN102866214B CN 201210392697 CN201210392697A CN102866214B CN 102866214 B CN102866214 B CN 102866214B CN 201210392697 CN201210392697 CN 201210392697 CN 201210392697 A CN201210392697 A CN 201210392697A CN 102866214 B CN102866214 B CN 102866214B
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Abstract
The invention discloses a method for detecting content of triethylamine in gas-phase condensed recovery liquid obtained from SAPO34 preparation. The method comprises the steps as follows: (1) preparing ethanol/triethylamine standard solution; (2) preparing liquid to be detected: collecting the upper layer liquid of the gas-phase condensed recovery liquid obtained from SAPO34 preparation, and adding ethanol with amount of 0.225- 0.9 times of mass, or collect in the lower layer liquid of the gas-phase condensed recovery liquid obtained from SAPO34 preparation, and adding ethanol with amount of 0.025-0.1 times of mass; (3) operating a gas chromatograph; (4) detecting correcting factor of the standard solution; and (5) detecting peak areas of ethanol and triethylamine in the liquid to be detected, wherein the mass of triethylamine=correcting factor*(mass of ethanol/peak area of ethanol)*peak area of triethylamine. The method disclosed by the invention is simple, has few steps, is simple and convenient to operate, and is fast to learn; and the measurement can be simply carried out for less than 5 minutes each time; and the method provided by the invention is accurate; the triethylamine ethanol aqueous solution with known concentration can be calibrated, and the error is less than 2%.
Description
Technical field
The present invention relates to a kind of the detection and prepare the method that the SAPO34 vapor condensation reclaims triethylamine content in the liquid.
Background technology
The SAPO-34 molecular sieve is that U.S. combinating carbide company (UCC) is in the novel crystallization silicoaluminophosphamolecular molecular sieves (USP 4,440,871) of exploitation in 1984.This molecular sieve is by PO
2, AlO
2, SiO
2Three kinds of tetrahedrons interconnect and form, and anhydrous chemical composition can be expressed as: (Si
xAl
yP
z) O
2, x, y, z are respectively the mole fraction of Si, Al, P, and satisfy x+y+z=1.The SAPO-34 molecular sieve contains special octatomic ring channel architecture, and has proper acidic.At the MTO(methanol-to-olefins) in the reaction, can suppress the generation of higher olefins such as aromatic hydrocarbons effectively, the selection performance of low-carbon alkene ethene and propylene is reached more than 80%.In addition, the SAPO-34 molecular sieve also has excellent thermal stability and hydrothermal stability, can adapt to multiple commercial production condition.
At present, preparation SAPO-34 molecular sieve a kind of method comparatively commonly used is the aluminium source, and silicon source and phosphorus source are under the effect of template agent triethylamine, and crystallization grows into SAPO-34 under the certain condition.For example, Wei Fei etc. (CN 200510083114.8) are the template agent with the triethylamine, have invented the preparation method of load type silicon phoshporus aluminium molecular sieve.Liu Zhongmin etc. (CN 200610152273.3) are the template agent with the triethylamine, and quaternary ammonium salt is organic amine promoter, have invented a kind of method of fast synthetic SAPO-34 molecular sieve.Triethylamine has moderate harm toxicity, and respiratory tract is had strong impulse, can cause pulmonary edema even death after the suction.Oral corrosion oral cavity, esophagus and stomach.Eye and skin contact can cause chemical burn.In addition, triethylamine is inflammable and explosive fried material, and its volume explosion limits is 1.2%-8.0%.When mass preparation SAPO-34 molecular sieve, for the security of production environment, for the preparation cost of farthest preserving the ecological environment and reducing the SAPO-34 molecular sieve, need carry out recycling to reacted triethylamine.Finish in the SAPO-34 crystallization, reactor contains a large amount of triethylamines and water in the gas phase of reactor upper strata before beginning cooling.The steam of releasing uses heat interchanger that triethylamine and water condensation are got off and shift to be stored in the storage tank.The gas phase recovery liquid of triethylamine and water is divided into two-layer up and down automatically, and the mass content of triethylamine is about 90% in the upper solution, and the mass content of triethylamine is about 10% in lower floor's solution.Before the utilization again of triethylamine, need accurately to measure respectively the content of triethylamine in upper solution and the lower floor's solution.
Summary of the invention
The purpose of this invention is to provide simply, a kind of detection prepares the method that the SAPO34 vapor condensation reclaims triethylamine content in the liquid fast and accurately, for the utilization again of triethylamine provides support.
Technical scheme of the present invention is summarized as follows:
A kind of detection prepares the method that the SAPO34 vapor condensation reclaims triethylamine content in the liquid, comprises the steps:
(1) the preparation mass ratio is ethanol/triethylamine standard solution of 0.25～1:1;
(2) prepare liquid to be measured, get the upper strata liquid that preparation SAPO34 vapor condensation reclaims liquid, add 0.225～0.9 quality ethanol doubly; Or get the subnatant that preparation SAPO34 vapor condensation reclaims liquid, add 0.025～0.1 quality ethanol doubly;
(3) use gas chromatograph, select the HP-1 capillary column for use; FID is detecting device, 200～250 ℃ of detector temperatures; Post case constant temperature, 50～75 ℃ of post oven temperature, degree; 180～250 ℃ of injector temperature; Pressure 0.1～0.15MPa before the capillary column;
(4) correction factor of the described standard solution of mensuration, correction factor=(triethylamine quality/triethylamine peak area)/(ethanol quality/ethanol peak area);
(5) peak area of ethanol and triethylamine in the described liquid to be measured of mensuration; Triethylamine quality=correction factor * (ethanol quality/ethanol peak area) * triethylamine peak area.
Advantage of the present invention:
Method provided by the invention is very simple, and step is less, and is easy and simple to handle, and study is got up very fast.Method provided by the invention can be measured fast and prepare the method that the SAPO-34 vapor condensation reclaims triethylamine content in the liquid, and one-shot measurement only need be less than 5 minutes.Method provided by the invention very accurately, demarcate the triethylamine ethanol water of concentration known, error is less than 2%.
Embodiment
Below in conjunction with specific embodiment to further instruction of the present invention.
The triethylamine aqueous solution of retrieving is divided into two-layer up and down.Be mainly triethylamine in the upper solution, massfraction is about 90%.The content of triethylamine is less in lower floor's solution, and massfraction is about 10%.
Embodiment 1
A kind of detection prepares the method that the SAPO34 vapor condensation reclaims triethylamine content in the liquid, comprises the steps:
(1) ethanol/triethylamine standard solution of preparation 1:1,5g ethanol wherein, 5g triethylamine;
(2) prepare liquid to be measured, get the upper strata liquid 10g that preparation SAPO34 vapor condensation reclaims liquid, add 9g ethanol;
(3) use gas chromatograph, select the HP-1 capillary column for use; FID is detecting device, 200 ℃ of detector temperatures; Post case constant temperature, 50 ℃ of post oven temperature, degree; 200 ℃ of injector temperature; Pressure 0.1MPa before the capillary column;
(4) correction factor of the described standard solution of mensuration, correction factor=(triethylamine quality/triethylamine peak area)/(ethanol quality/ethanol peak area) measured three times, and averaged 0.604;
(5) peak area of ethanol and triethylamine in the described liquid to be measured of mensuration; Triethylamine quality=correction factor * (ethanol quality/ethanol peak area) * triethylamine peak area.Measure three times, 8.82g averages.
Demarcate the triethylamine aqueous solution of concentration known, verify that mensuration provided by the present invention prepares the accuracy that the SAPO-34 gas phase reclaims triethylamine content method in the liquid.
(1) triethylamine/ethanol standard solution of preparation 1:1,5g triethylamine wherein, 5g ethanol;
(2) take by weighing triethylamine 9.5g, take by weighing water 0.5g, be mixed into the triethylamine aqueous solution of concentration known, take by weighing ethanol 9.5g, mix with the triethylamine aqueous solution of concentration known, be mixed with solution to be measured;
(3) use gas chromatograph, select the HP-1 capillary column for use; FID is detecting device, 200 ℃ of detector temperatures; Post case constant temperature, 50 ℃ of post oven temperature, degree; 200 ℃ of injector temperature; Pressure 0.1MPa before the capillary column;
(4) correction factor of the described standard solution of mensuration, correction factor=(triethylamine quality/triethylamine peak area)/(ethanol quality/ethanol peak area) measured three times, and averaged 0.604;
(5) peak area of ethanol and triethylamine in the described liquid to be measured of mensuration; Triethylamine quality=correction factor * (ethanol quality/ethanol peak area) * triethylamine peak area is measured three times, and 9.41g averages.
Error 0.9%.
Embodiment 2
A kind of detection prepares the method that the SAPO34 vapor condensation reclaims triethylamine content in the liquid, comprises the steps:
(1) ethanol/triethylamine standard solution of preparation 0.25:1,3.75g ethanol wherein, 15g triethylamine;
(2) prepare liquid to be measured, get the upper strata liquid 10g that preparation SAPO34 vapor condensation reclaims liquid, add 2.25g ethanol;
(3) use gas chromatograph, select the HP-1 capillary column for use; FID is detecting device, 250 ℃ of detector temperatures; Post case constant temperature, 75 ℃ of post oven temperature, degree; 250 ℃ of injector temperature; Pressure 0.12MPa before the capillary column;
(4) correction factor of the described standard solution of mensuration, correction factor=(triethylamine quality/triethylamine peak area)/(ethanol quality/ethanol peak area) measured three times, and averaged 0.623;
(5) peak area of ethanol and triethylamine in the described liquid to be measured of mensuration; Triethylamine quality=correction factor * (ethanol quality/ethanol peak area) * triethylamine peak area is measured three times, and 8.84g averages.
Embodiment 3
A kind of detection prepares the method that the SAPO34 vapor condensation reclaims triethylamine content in the liquid, comprises the steps:
(1) ethanol/triethylamine standard solution of preparation 0.50:1,5g ethanol wherein, 10g triethylamine;
(2) prepare liquid to be measured, get the upper strata liquid 10g that preparation SAPO34 vapor condensation reclaims liquid, add 4.50g ethanol;
(3) use gas chromatograph, select the HP-1 capillary column for use; FID is detecting device, 225 ℃ of detector temperatures; Post case constant temperature, 60 ℃ of post oven temperature, degree; 180 ℃ of injector temperature; Pressure 0.15MPa before the capillary column;
(4) correction factor of the described standard solution of mensuration, correction factor=(triethylamine quality/triethylamine peak area)/(ethanol quality/ethanol peak area) measured three times, and averaged 0.613;
(5) peak area of ethanol and triethylamine in the described liquid to be measured of mensuration; Triethylamine quality=correction factor * (ethanol quality/ethanol peak area) * triethylamine peak area is measured three times, and 8.83g averages.
Embodiment 4
A kind of detection prepares the method that the SAPO34 vapor condensation reclaims triethylamine content in the liquid, comprises the steps:
(1) ethanol/triethylamine standard solution of preparation 1:1,5g ethanol wherein, 5g triethylamine;
(2) prepare liquid to be measured, get the subnatant 10g that preparation SAPO34 vapor condensation reclaims liquid, add 1g ethanol;
(3) use gas chromatograph, select the HP-1 capillary column for use; FID is detecting device, 250 ℃ of detector temperatures; Post case constant temperature, 75 ℃ of post oven temperature, degree; 180 ℃ of injector temperature; Pressure 0.15MPa before the capillary column;
(4) correction factor of the described standard solution of mensuration, correction factor=(triethylamine quality/triethylamine peak area)/(ethanol quality/ethanol peak area) measured three times, and averaged 0.604;
(5) peak area of ethanol and triethylamine in the described liquid to be measured of mensuration; Triethylamine quality=correction factor * (ethanol quality/ethanol peak area) * triethylamine peak area is measured three times, and 1.03g averages.
Embodiment 5
A kind of detection prepares the method that the SAPO34 vapor condensation reclaims triethylamine content in the liquid, comprises the steps:
(1) ethanol/triethylamine standard solution of preparation 0.25:1,3.75g ethanol wherein, 15g triethylamine;
(2) prepare liquid to be measured, get the subnatant 10g that preparation SAPO34 vapor condensation reclaims liquid, add 0.25g ethanol;
(3) use gas chromatograph, select the HP-1 capillary column for use; FID is detecting device, 225 ℃ of detector temperatures; Post case constant temperature, 50 ℃ of post oven temperature, degree; 200 ℃ of injector temperature; Pressure 0.13MPa before the capillary column;
(4) correction factor of the described standard solution of mensuration, correction factor=(triethylamine quality/triethylamine peak area)/(ethanol quality/ethanol peak area) measured three times, and averaged 0.623;
(5) peak area of ethanol and triethylamine in the described liquid to be measured of mensuration; Triethylamine quality=correction factor * (ethanol quality/ethanol peak area) * triethylamine peak area is measured three times, and 1.05g averages.
Embodiment 6
A kind of detection prepares the method that the SAPO34 vapor condensation reclaims triethylamine content in the liquid, comprises the steps:
(1) ethanol/triethylamine standard solution of preparation 0.5:1,5g ethanol wherein, 10g triethylamine;
(2) prepare liquid to be measured, get the subnatant 10g that preparation SAPO34 vapor condensation reclaims liquid, add 0.5g ethanol;
(3) use gas chromatograph, select the HP-1 capillary column for use; FID is detecting device, 200 ℃ of detector temperatures; Post case constant temperature, 60 ℃ of post oven temperature, degree; 250 ℃ of injector temperature; Pressure 0.10MPa before the capillary column;
(4) correction factor of the described standard solution of mensuration, correction factor=(triethylamine quality/triethylamine peak area)/(ethanol quality/ethanol peak area) measured three times, and averaged 0.613;
(5) peak area of ethanol and triethylamine in the described liquid to be measured of mensuration; Triethylamine quality=correction factor * (ethanol quality/ethanol peak area) * triethylamine peak area is measured three times, and 1.04g averages.
Claims (1)
1. one kind is detected the method for preparing triethylamine content in the SAPO34 vapor condensation recovery liquid, it is characterized in that comprising the steps:
(1) the preparation mass ratio is ethanol/triethylamine standard solution of 0.25～1:1;
(2) prepare liquid to be measured, get the upper strata liquid that preparation SAPO34 vapor condensation reclaims liquid, add 0.225～0.9 quality ethanol doubly; Or get the subnatant that preparation SAPO34 vapor condensation reclaims liquid, add 0.025～0.1 quality ethanol doubly;
(3) use gas chromatograph, select the HP-1 capillary column for use; FID is detecting device, 200～250 ℃ of detector temperatures; Post case constant temperature, 50～75 ℃ of post oven temperature, degree; 180～250 ℃ of injector temperature; Pressure 0.1～0.15MPa before the capillary column;
(4) correction factor of the described standard solution of mensuration, correction factor=(triethylamine quality/triethylamine peak area)/(ethanol quality/ethanol peak area);
(5) peak area of ethanol and triethylamine in the described liquid to be measured of mensuration; Triethylamine quality=correction factor * (ethanol quality/ethanol peak area) * triethylamine peak area.
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| CN101038272A (en) * | 2006-03-15 | 2007-09-19 | 山东华鲁恒升化工股份有限公司 | Detecting device and method for diethylamine and triethylamine product |
| CN101633508A (en) * | 2008-07-24 | 2010-01-27 | 中国石油化工股份有限公司 | SAPO-34 molecular sieve and synthesis method thereof |
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| CN101038272A (en) * | 2006-03-15 | 2007-09-19 | 山东华鲁恒升化工股份有限公司 | Detecting device and method for diethylamine and triethylamine product |
| CN101633508A (en) * | 2008-07-24 | 2010-01-27 | 中国石油化工股份有限公司 | SAPO-34 molecular sieve and synthesis method thereof |
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