CN106861773A - The method that the isomerization catalyst of carbon four is prepared using useless platinum based catalyst - Google Patents
The method that the isomerization catalyst of carbon four is prepared using useless platinum based catalyst Download PDFInfo
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- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/90—Regeneration or reactivation
- B01J23/96—Regeneration or reactivation of catalysts comprising metals, oxides or hydroxides of the noble metals
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- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
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- B01J38/00—Regeneration or reactivation of catalysts, in general
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Abstract
The invention discloses a kind of method for preparing the isomerization catalyst of carbon four using useless platinum based catalyst, it is related to technical field of petrochemical industry, comprises the following steps：(1) wash, (2) dry, calcining, (3) pickling, (4) regeneration.The present invention realizes the regeneration of useless platinum based catalyst, and the catalyst that the isomerization of carbon four prepares light aromatic hydrocarbons is obtained, in the case where the basis that selective catalysis efficiency reaches more than 90% is ensured, effectively reduce the acquisition cost of platinum based catalyst and mitigate the influence that discarded platinum based catalyst is caused to environment.
Description
Technical field：
The present invention relates to technical field of petrochemical industry, and in particular to one kind prepares the isomerization of carbon four using useless platinum based catalyst
The method of catalyst.
Background technology：
C-4-fraction is the mixture of the various hydro carbons containing four carbon atom, is mainly derived from generation in petroleum refining process
Refinery gas and petroleum cracking ethene by-product, be the basic chemical raw materials with potential value.Utilization to C-4-fraction,
One of which is exactly that heavy aromatics and light aromatic hydrocarbons are produced to the isomerization of carbon four, and the economic benefit of light aromatic hydrocarbons is higher than heavy aromatics, and sharp
The light aromatic hydrocarbons yield produced out with previous methods is relatively low, it is therefore desirable to carrys out selective isomerization by using catalyst and produces light virtue
Hydrocarbon.
Platinum based catalyst is the custom catalystses of the isomerization of carbon four, is 2-3 usually using the life-span, therefore is had every year big
The useless platinum based catalyst of amount is produced.If dealing with useless platinum based catalyst improperly, natural environment will be caused to have a strong impact on, while leading
Cause the serious waste of heavy metal resources.How effective recycling is carried out to useless platinum based catalyst, as current numerous enterprises
The great difficult problem for facing.Also, current heavy metal holds at high price, and considerably increases the production cost of platinum based catalyst.
The content of the invention：
The technical problems to be solved by the invention are to provide a kind of effective on the basis of catalyst efficiency is ensured
The method that the useless platinum based catalyst of utilization of reduces cost and mitigation environmental pollution prepares the isomerization catalyst of carbon four.
The technical problems to be solved by the invention are realized using following technical scheme：
The method that the isomerization catalyst of carbon four is prepared using useless platinum based catalyst, is comprised the following steps：
(1) wash：By in useless platinum based catalyst 40-50 DEG C of water of addition, insulated and stirred 1h adds builder, fully mixed
Continue to be heated to reflux state insulated and stirred 15min after conjunction, be then stored at room temperature 2h, be finally again heated to reflux state insulation
Stirring 15min, is cooled to stratification after room temperature, is filtered using filter paper after upper oil phase and suspension are removed, gained filter
Slag is rinsed twice with clear water；
(2) dry, calcine：Useless platinum based catalyst after washing is placed in 75-80 DEG C of baking oven and is dried, treat that water content is low
In calcining furnace being transferred to after 1%, and in calcining 3h at 450-500 DEG C；
(3) pickling：To be added in hydrochloric acid solution through the useless platinum based catalyst after calcining, 1h is stood after being sufficiently mixed, then add
Heat first uses nanofiltration membrane to reflux state insulation mixing 15min after being cooled to room temperature, and resulting solution recycles emulsion
Film is processed, and obtains final product platinum ion solution；
(4) regenerate：Gained platinum ion solution is carried out into concentration calibration, and according to the composition needs of the isomerization catalyst of carbon four
Addition platinum chloride, new platinum based catalyst is obtained finally by coprecipitation.
The builder is made up of the raw material of following parts by weight：Water-based acrylic resin 3-6 parts, pre-gelatinized starch 3-6
Part, polyethylene glycol oxide 2-4 parts, PVPP 2-4 parts, rilanit special 1-2 parts, turpentine oil 1-2 parts, N- methylol acryloyls
Amine 0.5-1 parts, asbestos wool 0.5-1 parts, HPMA 0.2-0.5 parts, sodium abietate 0.2-0.5 parts, water 40-50 parts,
Its preparation method is：To addition rilanit special, turpentine oil and N hydroxymethyl acrylamide in polyethylene glycol oxide, after being sufficiently mixed
In microwave treatment 5min under microwave frequency 2450MHz, power 700W, add pre-gelatinized starch, asbestos wool and hydrolyze poly- Malaysia
Acid anhydrides, microwave treatment 5min is continued after being well mixed, and water, water-based acrylic resin, PVPP and pine are then added while hot
Fragrant acid sodium, is transferred in 0-5 DEG C of environment after being sufficiently mixed and stands 3h, and finally heated to reflux state insulation mixing 15min, gained is mixed
In compound feeding spray dryer, dry gained particle and be made powder through micronizer.
The water-based acrylic resin is formed by acrylic resin is modified, and its preparation method is：To 15-20 parts of acrylic acid tree
Cosmetics adds 1-2 parts of cetostearyl alcohol, 0.5-1 parts of sodium carboxymethylcellulose and 0.1-0.2 parts of titanate coupling agent in end, fully
Mixing continues microwave treatment 5min after microwave treatment 5min under microwave frequency 2450MHz, power 700W after standing 30min, then
Add 0.5-1 part PAMA and 0.5-1 parts of HPO, it is well mixed after microwave treatment 5min again, so
Cooled with the speed of 10-15 DEG C/min afterwards, be incubated after temperature is down to 0-5 DEG C and stand 1h, be subsequently added 60-80 parts of boiling
Water, naturally cools to room temperature after being sufficiently mixed, finally by gained mixture feeding spray dryer, dry gained particle through super
Atomizer is made powder.
By the addition of builder, the oily matter and dust adhered on useless platinum based catalyst are effectively removed, and through standing
It is present on water phase with suspended pattern afterwards, acquisition can be filtered through a water by filter paper after removing upper oil phase and suspension
Useless platinum based catalyst after washing.
The emulsion liquid film be with di-(2-ethylhexyl)phosphoric acid ester as membrane carrier, LMS-2 as surfactant, four chlorinations
Carbon is membrane solvent, NaOH is made for phase in film.
The useless platinum based catalyst is 1 with the weight ratio of hydrochloric acid solution:3-5.
The mass concentration of the hydrochloric acid solution is 20%.
The beneficial effects of the invention are as follows：The present invention realizes the regeneration of useless platinum based catalyst, and the isomery of carbon four is obtained
Change the catalyst for preparing light aromatic hydrocarbons, in the case where the basis that selective catalysis efficiency reaches more than 90% is ensured, effectively reduce platinum base catalysis
The influence that the acquisition cost of agent and the discarded platinum based catalyst of mitigation are caused to environment；Wherein by NF membrane and the association of emulsion liquid film
Same-action, effectively catching platinum ion, rejection reaches more than 99.5%.
Specific embodiment：
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment 1
(1) wash：By in useless platinum based catalyst 40-50 DEG C of water of addition, insulated and stirred 1h adds builder, fully mixed
Continue to be heated to reflux state insulated and stirred 15min after conjunction, be then stored at room temperature 2h, be finally again heated to reflux state insulation
Stirring 15min, is cooled to stratification after room temperature, is filtered using filter paper after upper oil phase and suspension are removed, gained filter
Slag is rinsed twice with clear water；
(2) dry, calcine：Useless platinum based catalyst after washing is placed in 75-80 DEG C of baking oven and is dried, treat that water content is low
In calcining furnace being transferred to after 1%, and in calcining 3h at 450-500 DEG C；
(3) pickling：5 times of hydrochloric acid solutions of the mass concentration of weight portion 20% will be added through the useless platinum based catalyst after calcining
In, 1h is stood after being sufficiently mixed, reflux state insulation mixing 15min is again heated to, first use NF membrane after being cooled to room temperature
Filtering, resulting solution recycles emulsion liquid film to be processed, and obtains final product platinum ion solution；
(4) regenerate：Gained platinum ion solution is carried out into concentration calibration, and according to the composition needs of the isomerization catalyst of carbon four
Addition platinum chloride, new platinum based catalyst is obtained finally by coprecipitation.
Wherein, emulsion liquid film be with di-(2-ethylhexyl)phosphoric acid ester as membrane carrier, LMS-2 as surfactant, tetrachloro
Change carbon is membrane solvent, NaOH is made for phase in film.
The preparation of builder：To 1 part of rilanit special, 1 part of turpentine oil and 0.5 part of N- hydroxyl of addition in 4 parts of polyethylene glycol oxides
Methacrylamide, is sufficiently mixed after microwave treatment 5min under microwave frequency 2450MHz, power 700W, adds 3 parts of pre- pastes
Change starch, 0.5 part of asbestos wool and 0.5 part of HPMA, microwave treatment 5min is continued after being well mixed, then add while hot
Enter 40 parts of water, 3 parts of water-based acrylic resins, 3 parts of PVPPs and 0.3 part of sodium abietate, 0-5 DEG C of ring is transferred to after being sufficiently mixed
3h is stood in border, it is finally heated to reflux state insulation mixing 15min, in gained mixture feeding spray dryer, dry institute
Obtain particle and be made powder through micronizer.
The preparation of water-based acrylic resin：To 1 part of cetostearyl alcohol, 0.5 part of carboxylic of addition in 20 parts of acrylic resin powders
Sodium carboxymethylcellulose pyce and 0.1 part of titanate coupling agent, are sufficiently mixed at microwave under microwave frequency 2450MHz, power 700W
Reason 5min, microwave treatment 5min is continued after standing 30min, adds 0.5 part of PAMA and 0.5 part of hydrogenated palm
Oil, microwave treatment 5min again after being well mixed, is then cooled with the speed of 10-15 DEG C/min, treats that temperature is down to 0-5 DEG C
Insulation afterwards stands 1h, is subsequently added 80 parts of boiling water, and room temperature is naturally cooled to after being sufficiently mixed, and finally sends into gained mixture and sprays
In mist drying machine, dry gained particle and be made powder through micronizer.
Embodiment 2
(1) wash：By in useless platinum based catalyst 40-50 DEG C of water of addition, insulated and stirred 1h adds builder, fully mixed
Continue to be heated to reflux state insulated and stirred 15min after conjunction, be then stored at room temperature 2h, be finally again heated to reflux state insulation
Stirring 15min, is cooled to stratification after room temperature, is filtered using filter paper after upper oil phase and suspension are removed, gained filter
Slag is rinsed twice with clear water；
(2) dry, calcine：Useless platinum based catalyst after washing is placed in 75-80 DEG C of baking oven and is dried, treat that water content is low
In calcining furnace being transferred to after 1%, and in calcining 3h at 450-500 DEG C；
(3) pickling：5 times of hydrochloric acid solutions of the mass concentration of weight portion 20% will be added through the useless platinum based catalyst after calcining
In, 1h is stood after being sufficiently mixed, reflux state insulation mixing 15min is again heated to, first use NF membrane after being cooled to room temperature
Filtering, resulting solution recycles emulsion liquid film to be processed, and obtains final product platinum ion solution；
(4) regenerate：Gained platinum ion solution is carried out into concentration calibration, and according to the composition needs of the isomerization catalyst of carbon four
Addition platinum chloride, new platinum based catalyst is obtained finally by coprecipitation.
The preparation of builder：To 1 part of rilanit special, 1 part of turpentine oil and 0.5 part of N- hydroxyl of addition in 4 parts of polyethylene glycol oxides
Methacrylamide, is sufficiently mixed after microwave treatment 5min under microwave frequency 2450MHz, power 700W, adds 5 parts of pre- pastes
Change starch, 0.5 part of asbestos wool and 0.5 part of HPMA, microwave treatment 5min is continued after being well mixed, then add while hot
Enter 50 parts of water, 3 parts of water-based acrylic resins, 3 parts of PVPPs and 0.3 part of sodium abietate, 0-5 DEG C of ring is transferred to after being sufficiently mixed
3h is stood in border, it is finally heated to reflux state insulation mixing 15min, in gained mixture feeding spray dryer, dry institute
Obtain particle and be made powder through micronizer.
The preparation of water-based acrylic resin：To 1 part of cetostearyl alcohol, 1 part of carboxylic first of addition in 20 parts of acrylic resin powders
Base sodium cellulosate and 0.2 part of titanate coupling agent, are sufficiently mixed after microwave treatment under microwave frequency 2450MHz, power 700W
5min, microwave treatment 5min is continued after standing 30min, adds 0.5 part of PAMA and 0.5 part of hydrogenated palm
Oil, microwave treatment 5min again after being well mixed, is then cooled with the speed of 10-15 DEG C/min, treats that temperature is down to 0-5 DEG C
Insulation afterwards stands 1h, is subsequently added 80 parts of boiling water, and room temperature is naturally cooled to after being sufficiently mixed, and finally sends into gained mixture and sprays
In mist drying machine, dry gained particle and be made powder through micronizer.
Reference examples 1
(1) wash：By in useless platinum based catalyst 40-50 DEG C of water of addition, insulated and stirred 1h adds builder, fully mixed
Continue to be heated to reflux state insulated and stirred 15min after conjunction, be then stored at room temperature 2h, be finally again heated to reflux state insulation
Stirring 15min, is cooled to stratification after room temperature, is filtered using filter paper after upper oil phase and suspension are removed, gained filter
Slag is rinsed twice with clear water；
(2) dry, calcine：Useless platinum based catalyst after washing is placed in 75-80 DEG C of baking oven and is dried, treat that water content is low
In calcining furnace being transferred to after 1%, and in calcining 3h at 450-500 DEG C；
(3) pickling：5 times of hydrochloric acid solutions of the mass concentration of weight portion 20% will be added through the useless platinum based catalyst after calcining
In, 1h is stood after being sufficiently mixed, reflux state insulation mixing 15min is again heated to, first use NF membrane after being cooled to room temperature
Filtering, resulting solution recycles emulsion liquid film to be processed, and obtains final product platinum ion solution；
(4) regenerate：Gained platinum ion solution is carried out into concentration calibration, and according to the composition needs of the isomerization catalyst of carbon four
Addition platinum chloride, new platinum based catalyst is obtained finally by coprecipitation.
The preparation of builder：To 1 part of rilanit special, 1 part of turpentine oil and 0.5 part of N- hydroxyl of addition in 4 parts of polyethylene glycol oxides
Methacrylamide, is sufficiently mixed after microwave treatment 5min under microwave frequency 2450MHz, power 700W, adds 5 parts of pre- pastes
Change starch, 0.5 part of asbestos wool and 0.5 part of HPMA, microwave treatment 5min is continued after being well mixed, then add while hot
Enter 50 parts of water, 3 parts of PVPPs and 0.3 part of sodium abietate, be transferred to after being sufficiently mixed in 0-5 DEG C of environment and stand 3h, finally plus
Heat in gained mixture feeding spray dryer, dries gained particle through micronizer to reflux state insulation mixing 15min
It is made powder.
Reference examples 2
(1) wash：By in useless platinum based catalyst 40-50 DEG C of water of addition, insulated and stirred 1h continues to be heated to reflux state guarantor
Temperature stirring 15min, is then stored at room temperature 2h, reflux state insulated and stirred 15min is finally again heated to, after being cooled to room temperature
Stratification, is filtered after upper oil phase and suspension are removed using filter paper, and gained filter residue is rinsed twice with clear water；
(2) dry, calcine：Useless platinum based catalyst after washing is placed in 75-80 DEG C of baking oven and is dried, treat that water content is low
In calcining furnace being transferred to after 1%, and in calcining 3h at 450-500 DEG C；
(3) pickling：5 times of hydrochloric acid solutions of the mass concentration of weight portion 20% will be added through the useless platinum based catalyst after calcining
In, 1h is stood after being sufficiently mixed, reflux state insulation mixing 15min is again heated to, first use NF membrane after being cooled to room temperature
Filtering, resulting solution recycles emulsion liquid film to be processed, and obtains final product platinum ion solution；
(4) regenerate：Gained platinum ion solution is carried out into concentration calibration, and according to the composition needs of the isomerization catalyst of carbon four
Addition platinum chloride, new platinum based catalyst is obtained finally by coprecipitation.
Embodiment 3
Equivalent embodiment 1, embodiment 2, reference examples 1 and the made new platinum based catalyst of reference examples 2 are used for equivalent carbon four different
Structure produces light aromatic hydrocarbons, and determines the selective catalysis efficiency of made new platinum based catalyst and by the preparation method to platinum ion
The rate of recovery, as a result as shown in table 1.
The catalytic efficiency and the platinum ion rate of recovery of the made new platinum based catalyst of table 1
| Project | Embodiment 1 | Embodiment 2 | Reference examples 1 | Reference examples 2 |
| Selective catalysis efficiency/% | 92.93 | 93.41 | 80.24 | 65.32 |
| The platinum ion rate of recovery/% | 99.52 | 99.58 | 76.17 | 52.06 |
Find after testing, embodiment 1 and the made selective catalysis efficiency of embodiment 2 reach more than 90%, and in new platinum base
The rate of recovery in the preparation process of catalyst to platinum ion reaches more than 99.5%.
General principle of the invention and principal character and advantages of the present invention has been shown and described above.The technology of the industry
Personnel it should be appreciated that the present invention is not limited to the above embodiments, simply explanation described in above-described embodiment and specification this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appending claims and its
Equivalent thereof.
Claims (6)
1. the method for preparing the isomerization catalyst of carbon four using useless platinum based catalyst, it is characterised in that comprise the following steps：
(1) wash：By in useless platinum based catalyst 40-50 DEG C of water of addition, insulated and stirred 1h adds builder, after being sufficiently mixed
Continue to be heated to reflux state insulated and stirred 15min, be then stored at room temperature 2h, be finally again heated to reflux state insulated and stirred
15min, is cooled to stratification after room temperature, is filtered using filter paper after upper oil phase and suspension are removed, and gained filter residue is used
Clear water is rinsed twice；
(2) dry, calcine：Useless platinum based catalyst after washing is placed in 75-80 DEG C of baking oven and is dried, treat that water content is less than
It is transferred in calcining furnace after 1%, and in calcining 3h at 450-500 DEG C；
(3) pickling：To be added in hydrochloric acid solution through the useless platinum based catalyst after calcining, 1h is stood after being sufficiently mixed, be again heated to
Reflux state insulation mixing 15min, nanofiltration membrane is first used after being cooled to room temperature, and resulting solution recycles emulsion liquid film to enter
Row treatment, obtains final product platinum ion solution；
(4) regenerate：Gained platinum ion solution is carried out into concentration calibration, and addition is needed according to the composition of the isomerization catalyst of carbon four
Platinum chloride, new platinum based catalyst is obtained finally by coprecipitation.
2. the method that the useless platinum based catalyst of utilization according to claim 1 prepares the isomerization catalyst of carbon four, its feature exists
In the builder is made up of the raw material of following parts by weight：Water-based acrylic resin 3-6 parts, pre-gelatinized starch 3-6 parts, it is poly-
Ethylene oxide 2-4 parts, PVPP 2-4 parts, rilanit special 1-2 parts, turpentine oil 1-2 parts, N hydroxymethyl acrylamide
0.5-1 parts, asbestos wool 0.5-1 parts, HPMA 0.2-0.5 parts, sodium abietate 0.2-0.5 parts, water 40-50 parts, its
Preparation method is：To rilanit special, turpentine oil and N hydroxymethyl acrylamide is added in polyethylene glycol oxide, be sufficiently mixed after
Microwave treatment 5min under microwave frequency 2450MHz, power 700W, adds pre-gelatinized starch, asbestos wool and hydrolyzed polymaleic anhydride
Acid anhydride, microwave treatment 5min is continued after being well mixed, and water, water-based acrylic resin, PVPP and rosin are then added while hot
Sour sodium, is transferred in 0-5 DEG C of environment after being sufficiently mixed and stands 3h, finally heated to reflux state insulation mixing 15min, gained mixing
In thing feeding spray dryer, dry gained particle and be made powder through micronizer.
3. the method that the useless platinum based catalyst of utilization according to claim 2 prepares the isomerization catalyst of carbon four, its feature exists
In：The water-based acrylic resin is formed by acrylic resin is modified, and its preparation method is：To 15-20 parts of acrylic resin powder
1-2 parts of cetostearyl alcohol, 0.5-1 parts of sodium carboxymethylcellulose and 0.1-0.2 parts of titanate coupling agent are added in end, is sufficiently mixed
After microwave treatment 5min under microwave frequency 2450MHz, power 700W, microwave treatment 5min is continued after standing 30min, added
0.5-1 parts of PAMA and 0.5-1 parts of HPO, microwave treatment 5min again after being well mixed, then with
The speed of 10-15 DEG C/min cools, and is incubated after temperature is down to 0-5 DEG C and stands 1h, is subsequently added 60-80 parts of boiling water, fills
Point mixing after naturally cool to room temperature, finally will gained mixture send into spray dryer in, dry gained particle through Ultramicro-powder
Broken machine is made powder.
4. the method that the useless platinum based catalyst of utilization according to claim 1 prepares the isomerization catalyst of carbon four, its feature exists
In：The emulsion liquid film be with di-(2-ethylhexyl)phosphoric acid ester as membrane carrier, LMS-2 as surfactant, carbon tetrachloride be
Membrane solvent, NaOH are made for phase in film.
5. the method that the useless platinum based catalyst of utilization according to claim 1 prepares the isomerization catalyst of carbon four, its feature exists
In：The useless platinum based catalyst is 1 with the weight ratio of hydrochloric acid solution:3-5.
6. the method that the useless platinum based catalyst of utilization according to claim 1 prepares the isomerization catalyst of carbon four, its feature exists
In：The mass concentration of the hydrochloric acid solution is 20%.
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| CN108286208A (en) * | 2018-01-26 | 2018-07-17 | 刘成旭 | A method of improving paper strength using nano combined intercalation material |
| CN108913518A (en) * | 2018-06-12 | 2018-11-30 | 安徽省金裕皖酒业有限公司 | A kind of liquor aging method for using for reference the new vinegar after-ripening technique of mature vinegar |
| CN109046343A (en) * | 2018-08-29 | 2018-12-21 | 陕西瑞科新材料股份有限公司 | A kind of platinized asbestos catalyst spheres and preparation method thereof for gas phase hydrogenation |
| CN109046343B (en) * | 2018-08-29 | 2021-07-13 | 陕西瑞科新材料股份有限公司 | Platinum asbestos catalyst ball for gas phase hydrogenation and preparation method thereof |
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