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CN107694544A - The preparation method of ethene efficient molecular sieve - Google Patents

The preparation method of ethene efficient molecular sieve Download PDF

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Publication number
CN107694544A
CN107694544A CN201710945961.3A CN201710945961A CN107694544A CN 107694544 A CN107694544 A CN 107694544A CN 201710945961 A CN201710945961 A CN 201710945961A CN 107694544 A CN107694544 A CN 107694544A
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China
Prior art keywords
molecular sieve
powder
preparation
ethene
parts
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CN201710945961.3A
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Chinese (zh)
Inventor
甘成模
黄德金
甘玲
甘宇
张艳稻
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Jiangxi Pingxiang Chengyu Ceramic Co Ltd
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Jiangxi Pingxiang Chengyu Ceramic Co Ltd
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Priority to CN201710945961.3A priority Critical patent/CN107694544A/en
Publication of CN107694544A publication Critical patent/CN107694544A/en
Pending legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28016—Particle form
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12—Naturally occurring clays or bleaching earth
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16—Alumino-silicates
    • B01J20/165—Natural alumino-silicates, e.g. zeolites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16—Alumino-silicates
    • B01J20/18—Synthetic zeolitic molecular sieves
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C11/00—Aliphatic unsaturated hydrocarbons
    • C07C11/02—Alkenes
    • C07C11/04—Ethylene
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/46—Materials comprising a mixture of inorganic and organic materials

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

The invention discloses a kind of preparation method of ethene efficient molecular sieve, comprise the following steps：1）The raw material of following parts by weight is mixed with mixed powder：80 90 parts of natural zeolite, 10 20 parts of natural clay, 5 20 parts of native cellulose；2）In step 1）Add water in the mixed powder of preparation to stir, molecular sieve biscuit is made in extrusion or granulating and forming；3）By the molecular sieve biscuit naturally dry of preparation, drying, roasting, it can be prepared by ethene molecular sieve, the present invention has is more than more than 2 percentage points than conventional molecular sieve absorption property, and crush strength is high, and falling powder degree is low, the advantages of loadings are few, and adsorption cycle is long, the recovery time is short, molecular sieve service life is higher than more than 1 year.

Description

The preparation method of ethene efficient molecular sieve
Technical field
The present invention relates to technical field of molecular sieve, is especially a kind of preparation method of ethene efficient molecular sieve.
Background technology
Ethene is the basic material of petrochemical industry, and production technology is the core technology of petrochemical industry；Ethylene unit is also stone The core apparatus of oily chemical industry, the production technology level and production scale of ethene are even more to indicate a country in petrochemistry The development level of industrial circle.
Estimate according to Global Oil chemical industry, current global ethylene volume breach is up to 50,000,000 tons.It is special to research and develop large-scale ethene The technology of molecular sieve, it is that we manufacture a responsibility of molecular sieve people, and a harvest.Because the volume production of traditional sex ethylene limits Degree, domestic is all the device industrial condition within 1,000,000 tons/year at present.It is near to develop more than 1,000,000 tons/year of ethylene production line Phase domestic existing 8 project verifications, 5 sections between building and going into operation.Therefore, the quality of molecular sieve is improved, improves the skill of production technology Art, research and develop energy-efficient ethene and have great importance with molecular sieve.
The content of the invention
The technical problems to be solved by the invention are the shortcomings that overcoming above prior art：One kind is provided and compares conventional molecular Sieve absorption property and be more than more than 2 percentage points, crush strength is high, and falling powder degree is low, and loadings are few, adsorption cycle is long, regeneration when Between short, molecular sieve service life higher than the ethene efficient molecular sieve of more than 1 year preparation method.
The technical solution of the present invention is as follows：A kind of preparation method of ethene efficient molecular sieve, comprises the following steps：
1）The raw material of following parts by weight is mixed with mixed powder：Natural zeolite 80-90 parts, natural clay 10-20 parts, naturally Cellulose 5-20 parts；
2）In step 1）The water that weight is mixed powder gross weight 20-35% is added in the mixed powder of preparation to stir, and extrusion or is made Molecular sieve biscuit is made in grain shaping；
3）By the molecular sieve biscuit naturally dry of preparation, 1-2h is then dried at a temperature of 150-200 DEG C, then at 500-700 DEG C Roasting temperature 0.5-2.5h, you can obtained ethene molecular sieve.
Preferred, step 1 as raw material composition）Described in mixed powder be made up of the raw material of following parts by weight：Natural boiling Stone 80-85 parts, natural clay 15-20 parts, native cellulose 6-12 parts.
The natural zeolite is one or both of clinoptilolite powder, modenite powder, and particle diameter is less than 500 mesh.
The natural clay is the one or more in attapulgite powder, kaolin powder, Yang earthenware soil powder, sepiolite powder.
In order to reach Performance optimization, the attapulgite powder, kaolin powder, the particle diameter of Yang earthenware soil powder are less than 500 mesh, institute The particle diameter for stating sepiolite powder is less than 600 mesh.
The native cellulose is sodium carboxymethylcellulose, SG natural plant gum, the one or more of Guangxi myrica extract.
As optimization, the temperature of the roasting is 570-610 DEG C.
The beneficial effects of the invention are as follows：It is a kind of by used in traditional 500,000 tons/year of ethylene units the invention reside in providing In four groups of molecular sieves, the preparation method for the efficient molecular sieve applied in 100-300 ten thousand tons of six groups of devices of 1 year is lifted.This hair Bright molecular sieve pH value is 7-8, and exchange degree is more than 45, and equilibrium water absorption is more than 22%, and rate of wear is less than 0.10, crush strength 60-100N, service life are more than 5-8.The molecular sieve of the present invention is also equipped with advantages below：The main raw material(s) of 3A molecular sieves is complete Portion derives from natural material, adds adsorption capacity, also improves service life.The absorption duct of molecular sieve is flourishing, absorption point It is fairly obvious from effect.The product of natural material synthesis, falling powder degree is very low, is not burst using process broken, technique will not be frozen It is stifled.Molecular sieve after use, scrap processing conveniently, it is harmless to plant and water source with garbage loading embeading.
Embodiment
The present invention is described in further details with specific embodiment below, but the present invention is not only limited in detail below in fact Apply example.
Embodiment 1
By clinoptilolite powder 82kg, attapulgite powder 8kg, kaolin powder 10kg, sodium carboxymethylcellulose 8kg are mixed to prepare mixing Powder, water 32kg is added to be granulated after mixing 60 minutes with mixed powder；The particle made is dried into surface, summer and autumn day 12h is best, Winter-Spring day 48h, then can be prepared by molecular sieve through medium temperature 200 DEG C of drying 2h, 600 DEG C of roasting 2h.
The molecular sieve items technical performance obtained：Static Water absorption >=23%, Dynamic Water absorption >=21.6%, ethylene absorption Amount≤2.1%, crush strength 60-100N, rate of wear 0.10%.
Embodiment 2
By modenite powder 40kg, clinoptilolite powder 40kg, attapulgite powder 10kg, kaolin powder 10kg, carboxymethyl cellulose Sodium 7kg is mixed to prepare mixed powder, adds water 30kg to be granulated after mixing 60 minutes with mixed powder；The particle made is dried into surface, summer Autumn, 12h was best, Winter-Spring day 48h, then can be prepared by molecular sieve through medium temperature 200 DEG C of drying 2h, 610 DEG C of roasting 2.5h.
The indices performance of institute's acquisition molecular sieve：Molecular sieve Static Water absorption >=22.6%, Dynamic Water absorption >=21.2%, Ethylene absorption amount≤1.96%, crush strength 65-110N, rate of wear≤0.09%.
Embodiment 3
By modenite powder 30kg, clinoptilolite powder 50kg, attapulgite powder 5kg, kaolin powder 5kg, sepiolite powder 6kg, carboxylic The mixed powder that average grain diameter is 600-700 mesh is made in sodium carboxymethylcellulose pyce 7kg mixed grindings, adds water 30kg to mix 60 with mixed powder It is granulated after minute；The particle made is dried into surface, summer and autumn day 12h is best, Winter-Spring day 48h, then through 200 DEG C of medium temperature drying 2h, 610 DEG C of roasting 2.5h can be prepared by molecular sieve.
Institute's acquisition molecular sieve indices performance：Molecular sieve Static Water absorption >=21.72%, Dynamic Water absorption >=20.3%, Ethylene absorption amount≤2.56%, crush strength >=70-120N, rate of wear≤0.08%.
Embodiment 4
By modenite powder 32kg, clinoptilolite powder 50kg, kaolin powder 10kg, sepiolite powder 6kg, Guangxi myrica extract 6kg The mixed powder that average grain diameter is 600-700 mesh is made in mixed grinding, adds water 30kg to be granulated after mixing 60 minutes with mixed powder；It will make Good particle dries surface, and summer and autumn day 12h is best, Winter-Spring day 48h, then is through medium temperature 200 DEG C of drying 2h, 570 DEG C of roasting 2.5h Molecular sieve can be made.
Institute's acquisition molecular sieve indices performance：Molecular sieve Static Water absorption >=23%, Dynamic Water absorption >=21.8%, ethene Adsorbance≤2.3%, crush strength >=30-50N, rate of wear≤0.20%.
Embodiment 5
By modenite powder 85kg, kaolin powder 6kg, Yang earthenware soil powder 5kg, sepiolite powder 6kg, Guangxi myrica extract 6kg mixing The mixed powder that average grain diameter is 600-700 mesh is made in grinding, adds water 30kg to be granulated after mixing 60 minutes with mixed powder；By what is made Particle dries surface, and summer and autumn day 12h is best, Winter-Spring day 48h, then through 200 DEG C of drying 2h of medium temperature, 570 DEG C are calcined 2.5h and can make Obtain molecular sieve.
Institute's acquisition molecular sieve indices performance：Molecular sieve Static Water absorption >=22.71%, Dynamic Water absorption >=21.40%, Ethylene absorption amount≤2.6%, crush strength >=60-100N, rate of wear≤0.13%.
According to above-mentioned it is demonstrated experimentally that the spherical or strip particle molecular sieve performance index of high-efficiency adsorbent is fully able to practicality In the large-scale plant technique of ten thousand tons/year of production ethylene volumes of 100-300.Performance indications are better than traditional 3A molecular sieves more than 20% substantially.
It the above is only the feature implementation example of the present invention, the scope of the present invention be not limited in any way.It is all to use together The technical scheme formed Deng exchange or equivalence replacement, all falls within rights protection scope of the present invention.

Claims (7)

  1. A kind of 1. preparation method of ethene efficient molecular sieve, it is characterised in that：Comprise the following steps：
    1）The raw material of following parts by weight is mixed with mixed powder：Natural zeolite 80-90 parts, natural clay 10-20 parts, naturally Cellulose 5-20 parts；
    2）In step 1）The water that weight is mixed powder gross weight 20-35% is added in the mixed powder of preparation to stir, and extrusion or is made Molecular sieve biscuit is made in grain shaping；
    3）By the molecular sieve biscuit naturally dry of preparation, 1-2h is then dried at a temperature of 150-200 DEG C, then at 500-700 DEG C Roasting temperature 0.5-2.5h, you can obtained ethene molecular sieve.
  2. 2. the preparation method of ethene efficient molecular sieve according to claim 1, it is characterised in that：Step 1）Described in mix Powder is closed to be made up of the raw material of following parts by weight：Natural zeolite 80-85 parts, natural clay 15-20 parts, native cellulose 6-12 Part.
  3. 3. the preparation method of ethene efficient molecular sieve according to claim 1 or 2, it is characterised in that：The natural boiling Stone is one or both of clinoptilolite powder, modenite powder.
  4. 4. the preparation method of ethene efficient molecular sieve according to claim 1 or 2, it is characterised in that：It is described natural glutinous Soil is attapulgite powder, the one or more in kaolin powder, Yang earthenware soil powder, sepiolite powder.
  5. 5. the preparation method of ethene efficient molecular sieve according to claim 4, it is characterised in that：The attapulgite Powder, kaolin powder, the particle diameter of Yang earthenware soil powder are less than 500 mesh, and the particle diameter of the sepiolite powder is less than 600 mesh.
  6. 6. the preparation method of ethene efficient molecular sieve according to claim 1 or 2, it is characterised in that：It is described natural fine Dimension element is sodium carboxymethylcellulose, SG natural plant gum, the one or more of Guangxi myrica extract.
  7. 7. the preparation method of ethene efficient molecular sieve according to claim 1, it is characterised in that：The temperature of the roasting For 570-610 DEG C.
CN201710945961.3A 2017-10-12 2017-10-12 The preparation method of ethene efficient molecular sieve Pending CN107694544A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109046237A (en) * 2018-09-19 2018-12-21 江西萍乡市成宇陶瓷有限责任公司 A kind of preparation method of multi-selection binding molecule sieve
CN109126693A (en) * 2018-09-19 2019-01-04 江西萍乡市成宇陶瓷有限责任公司 A kind of preparation method of more partial size binding molecule sieves
CN109173624A (en) * 2018-10-17 2019-01-11 江西萍乡市成宇陶瓷有限责任公司 A kind of preparation method of the molecular sieve sintered body for refrigeration machine
CN109529787A (en) * 2018-12-11 2019-03-29 彭钰晗 A kind of preparation method of formaldehyde absorbing molecular sieve
CN113697824A (en) * 2021-08-26 2021-11-26 中国地质科学院郑州矿产综合利用研究所 Preparation process and application of modified 3A molecular sieve

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1082000A (en) * 1993-07-23 1994-02-16 周玉芳 Natural zeolite molecular sieve and production method thereof
CN102806101A (en) * 2012-08-13 2012-12-05 西南化工研究设计院有限公司 Catalyst for preparing ethylene by conversion of ethanol and preparation method of catalyst
CN105174283A (en) * 2015-09-25 2015-12-23 萍乡市鑫陶化工填料有限公司 Special molecular sieve for acetylene gas and preparation method of special molecular sieve
CN105771884A (en) * 2016-05-03 2016-07-20 武汉科技大学 Molecular sieve composite material for adsorbing heavy metal in water and method for preparing molecular sieve composite material
CN106082256A (en) * 2016-07-25 2016-11-09 江西科帕克环保化工有限责任公司 The preparation method that ethylene is dedicated molecular sieve used

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1082000A (en) * 1993-07-23 1994-02-16 周玉芳 Natural zeolite molecular sieve and production method thereof
CN102806101A (en) * 2012-08-13 2012-12-05 西南化工研究设计院有限公司 Catalyst for preparing ethylene by conversion of ethanol and preparation method of catalyst
CN105174283A (en) * 2015-09-25 2015-12-23 萍乡市鑫陶化工填料有限公司 Special molecular sieve for acetylene gas and preparation method of special molecular sieve
CN105771884A (en) * 2016-05-03 2016-07-20 武汉科技大学 Molecular sieve composite material for adsorbing heavy metal in water and method for preparing molecular sieve composite material
CN106082256A (en) * 2016-07-25 2016-11-09 江西科帕克环保化工有限责任公司 The preparation method that ethylene is dedicated molecular sieve used

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109046237A (en) * 2018-09-19 2018-12-21 江西萍乡市成宇陶瓷有限责任公司 A kind of preparation method of multi-selection binding molecule sieve
CN109126693A (en) * 2018-09-19 2019-01-04 江西萍乡市成宇陶瓷有限责任公司 A kind of preparation method of more partial size binding molecule sieves
CN109126693B (en) * 2018-09-19 2021-11-05 江西萍乡市成宇陶瓷有限责任公司 Preparation method of multi-particle-size adsorption molecular sieve
CN109173624A (en) * 2018-10-17 2019-01-11 江西萍乡市成宇陶瓷有限责任公司 A kind of preparation method of the molecular sieve sintered body for refrigeration machine
CN109529787A (en) * 2018-12-11 2019-03-29 彭钰晗 A kind of preparation method of formaldehyde absorbing molecular sieve
CN113697824A (en) * 2021-08-26 2021-11-26 中国地质科学院郑州矿产综合利用研究所 Preparation process and application of modified 3A molecular sieve
CN113697824B (en) * 2021-08-26 2023-08-25 中国地质科学院郑州矿产综合利用研究所 Preparation process and application of modified 3A molecular sieve

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Application publication date: 20180216