CN106831369A - A kind of method of city organic sludge catalytic production ketone organic matter - Google Patents
A kind of method of city organic sludge catalytic production ketone organic matter Download PDFInfo
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- CN106831369A CN106831369A CN201710047679.3A CN201710047679A CN106831369A CN 106831369 A CN106831369 A CN 106831369A CN 201710047679 A CN201710047679 A CN 201710047679A CN 106831369 A CN106831369 A CN 106831369A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G99/00—Subject matter not provided for in other groups of this subclass
Abstract
The present invention relates to a kind of method of city organic sludge catalytic production ketone organic matter, the sludge of municipal sewage plant is taken, by hydrothermal pretreatment, ketone organic matter is produced using the method for addition catalyst.Specifically:Taking city organic sludge carries out hydrothermal pretreatment, regathers the black liquor of generation;By black liquor stored frozen;Then Zr (Y) FeO is preparedXCatalyst is simultaneously granulated, and obtains Zr (Y) FeOXThe particle of catalyst;Take Zr (Y) FeO of gainedXThe particle of catalyst and the black liquor of stored frozen are added in reactor, and being passed through nitrogen makes reactor pressurize;It is stirred again after reactor is heated, reaction a period of time;The liquid substance after reaction terminates finally is collected, ketone organic matter is obtained.
Description
Technical field
The present invention relates to the technical field of organic sludge catalysis, and in particular to a kind of city organic sludge catalytic production ketone
The method of organic matter.
Background technology
As Chinese society economy and the fast development of urbanization, urban population are skyrocketed through, the thing followed is
The discharge capacity of China's municipal sewage is growing day by day.Municipal sludge as the secondary product in sewage treatment plant's sewage disposal process,
As the quickening of Development of China's Urbanization is necessarily increased rapidly.The negative effect that municipal sewage and sludge are caused to environment also gradually causes
Global concern.
At present, development relative maturity of the developed country such as America and Europe in municipal sludge process field.However, according to the country
Relevant data analysis, the annual dewatered sludge amount of China alreadys exceed 32,000,000 tons, and at present still with annual 5%~10% speed
Degree increases.Therefore, how rationally, effectively reclaim the valuable material in sludge turned into we one very urgent ask
Topic.
The conventional method of China's treatment municipal sludge mainly has landfill, burning and recycling.Using the side of landfill
Method treatment municipal sludge environmental pollution is serious, the moisture meeting osmosis pollution underground water in sludge, and valuable thing in sludge
Matter is not reclaimed completely;Big using the method treatment municipal sludge investment burned, equipment running cost is high, and can be produced during burning
The extremely toxic substances such as bioxin;Sludge such as making brick from sludge is processed using the recycling of sludge, is made because water content is higher in sludge
It is higher into brickmaking energy consumption and brick quality is relatively low, toxic and harmful can be produced in sintering procedure;It is agricultural to sludge after sludge composting
Quality requirement it is higher, and need to carry out high-temperature process to sludge before compost, processing cost is higher.
Above method treatment municipal sludge not only consumes substantial amounts of energy, and also results in serious environmental problems, such as air
Pollution, soil pollution and global warming etc..Due to containing organic compound enrich and valuable and battalion in municipal sludge
Element is supported, therefore, it is badly in need of providing a kind of method by the recovery of valuable substance in sludge at present.
The content of the invention
The present invention is carried out to solve the above problems, it is therefore intended that provide a kind of city organic sludge catalytic production
The method of ketone organic matter.
The invention provides a kind of method of city organic sludge catalytic production ketone organic matter, have the feature that,
Including:Step one, takes city organic sludge, and hydrothermal pretreatment is carried out at 200~400 DEG C, regathers life after hydrothermal pretreatment
Into black liquor;Step 2, stored frozen at least 24 hours at the black liquor of gained in step one is placed on into -20~0 DEG C;
Step 3, prepares Zr (Y)-FeOXCatalyst:By FeCl3Solution and ZrOCl2·8H2O solution is poured into and fully stirred in same container
Mix, be then filtrated to get Zr (Y)-FeOXCatalyst, in Zr (Y)-FeOXIn, Y is load ZrO2Mass fraction, Y value with added
Plus FeCl3Solution and ZrOCl2·8H2The amount of O solution is relevant, FeOXRepresent the oxide of iron;Step 4, by step 3 gained
Zr (Y)-FeOXCatalyst uses steam treatment at 500~800 DEG C;Step 5, by Zr (the Y)-FeO obtained by step 4XUrge
Agent is granulated under conditions of without any adhesive, crushed and sieves, and obtains Zr (Y)-FeOXThe particle of catalyst;Step
Six, the black liquor obtained by the particle and 1~5g step 2 of Zr (the Y)-FeOX catalyst obtained by 0~1g step 5 is added anti-
In answering device, and being passed through nitrogen makes the pressure of reactor reach 0~10MPa;Step 7,100~400 DEG C are heated to by reactor;
Step 8, the agitating device in reactor is opened, and reacts 0~4h;Step 9, the liquid after reaction terminates is collected by filter
Body material, obtains ketone organic matter.
In the method for the city organic sludge catalytic production ketone organic matter that the present invention is provided, can also have such
Feature:Wherein, in step one, the temperature of hydrothermal pretreatment is 300 DEG C.
In the method for the city organic sludge catalytic production ketone organic matter that the present invention is provided, can also have such
Feature:Wherein, in step 2, the temperature of stored frozen is -20 DEG C.
In the method for the city organic sludge catalytic production ketone organic matter that the present invention is provided, can also have such
Feature:Wherein, in step 3, mixing time is 0.5~120min.
In the method for the city organic sludge catalytic production ketone organic matter that the present invention is provided, can also have such
Feature:Wherein, in step 4, the temperature of steam treatment is 600 DEG C, and process time is 0~2h.
In the method for the city organic sludge catalytic production ketone organic matter that the present invention is provided, can also have such
Feature:Wherein, in step 5, screening obtains Zr (Y)-FeOXThe grain diameter of catalyst is 300~850mm.
In the method for the city organic sludge catalytic production ketone organic matter that the present invention is provided, can also have such
Feature:Wherein, in step 6, being passed through nitrogen makes the pressure of reactor reach 2MPa.
In the method for the city organic sludge catalytic production ketone organic matter that the present invention is provided, can also have such
Feature:Wherein, in step 7, the heating-up temperature of reactor is 250 DEG C.
In the method for the city organic sludge catalytic production ketone organic matter that the present invention is provided, can also have such
Feature:Wherein, in step 8, the reaction time is 2h.
The effect of invention and effect
The method of city organic sludge catalytic production ketone organic matter involved in the present invention, city organic sludge is passed through
Hydrothermal pretreatment, then by adding granular Zr (Y)-FeOXCatalyst is reacted, so that the organic dirt in city of the invention
The method of mud catalytic production ketone organic matter can obtain the ketone organic matter with high added value.The organic dirt in city of the invention
The method of mud catalytic production ketone organic matter has that technological process is short, working condition simple, recycle sludge in have it is high attached
The features such as value added ketone organic matter yield is high, preferably solves traditional approach pollution environment, valuable substance yield few
The problems such as, it is especially suitable for industrial application.
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, it is real below
Example is applied to be specifically addressed the method for city organic sludge catalytic production ketone organic matter of the present invention.
The city organic sludge in municipal sewage plant is taken as the experimental raw in embodiment.
<Embodiment one>
Step one, takes city organic sludge, and hydrothermal pretreatment is carried out at 300 DEG C, is generated after regathering hydrothermal pretreatment
Black liquor.
Step 2, by step one gained black liquor at -20 DEG C stored frozen 48 hours.
Step 3, takes the black liquor of stored frozen in 3.2g step 2, and measurement obtains the content of wherein ketone organic matter
It is 15.13mg/mL.During 3.2g black liquors are added into reactor, and being passed through nitrogen makes the pressure of reactor reach 2MPa.
Step 4,250 DEG C are heated to by reactor.
Step 5, the agitating device in reactor is opened, and reacts 2h.
Step 6, the liquid substance after reaction terminates is collected by filter, obtains ketone organic matter, and measurement obtains it and contains
Amount 15.89mg/mL.
From the foregoing, the ketone measured in the ketone content of organics measured in sample after reaction and the preceding sample of reaction has
Machine thing content is compared, and increased 5%.
<Embodiment two>
Step one, takes city organic sludge, and hydrothermal pretreatment is carried out at 300 DEG C, is generated after regathering hydrothermal pretreatment
Black liquor.
Step 2, by step one gained black liquor at -20 DEG C stored frozen 48 hours.
Step 3, prepares Zr (0)-FeOXCatalyst:By FeCl3Solution and ZrOCl2·8H2O solution pours into same container
Middle stirring, mixing time is 0.5~120min, is then filtrated to get Zr (0)-FeOXCatalyst.
Step 4, by Zr (the 0)-FeO obtained by step 3XCatalyst uses steam treatment 1h at 600 DEG C.
Step 5, by Zr (the 0)-FeO obtained by step 4XCatalyst granulates under conditions of without any adhesive,
Crush and sieve, obtain Zr (0)-FeO that particle diameter is 300~850mmXCatalyst granules.
Step 6, takes the black liquor of stored frozen in 3.2g step 2, and measurement obtains the content of wherein ketone organic matter
It is 15.27mg/mL.Take the particle of Zr (the 0)-FeOX catalyst obtained by 0.2g step 5.By 3.2g black liquors and 0.2gZr
(0) in the particle addition reactor of-FeOX catalyst, and being passed through nitrogen makes the pressure of reactor reach 2MPa.
Step 7,250 DEG C are heated to by reactor.
Step 8, the agitating device in reactor is opened, and reacts 2h.
Step 9, the liquid substance after reaction terminates is collected by filter, obtains ketone organic matter, and measurement obtains it and contains
It is 17.28mg/mL to measure.
From the foregoing, the ketone measured in the ketone content of organics measured in sample after reaction and the preceding sample of reaction has
Machine thing content is compared, and increased 15%.And compared to embodiment one, the ketone content of organics in the present embodiment substantially increases
Plus.
<Embodiment three>
Step one, takes city organic sludge, and hydrothermal pretreatment is carried out at 300 DEG C, is generated after regathering hydrothermal pretreatment
Black liquor.
Step 2, by step one gained black liquor at -20 DEG C stored frozen 48 hours.
Step 3, prepares Zr (7.7)-FeOXCatalyst:By FeCl3Solution and ZrOCl2·8H2O solution pours into same appearance
Stirred in device, mixing time is 0.5~120min, is then filtrated to get Zr (7.7)-FeOXCatalyst.
Step 4, by Zr (the 7.7)-FeO obtained by step 3XCatalyst uses steam treatment 1h at 600 DEG C.
Step 5, by Zr (the 7.7)-FeO obtained by step 4XCatalyst is made under conditions of without any adhesive
Grain, crush and sieve, obtain Zr (7.7)-FeO that particle diameter is 300~850mmXCatalyst granules.
Step 6, takes the black liquor of stored frozen in 3.2g step 2, and measurement obtains the content of wherein ketone organic matter
It is 15.09mg/mL.Take Zr (the 7.7)-FeO obtained by 0.2g step 5XThe particle of catalyst.By 3.2g black liquors and
The particle of 0.2gZr (7.7)-FeOX catalyst is added in reactor, and being passed through nitrogen makes the pressure of reactor reach 2MPa.
Step 7,250 DEG C are heated to by reactor.
Step 8, the agitating device in reactor is opened, and reacts 2h.
Step 9, the liquid substance after reaction terminates is collected by filter, obtains ketone organic matter, and measurement obtains it and contains
It is 27.92mg/mL to measure.
From the foregoing, the ketone measured in the ketone content of organics measured in sample after reaction and the preceding sample of reaction has
Machine thing content is compared, and increased 85%.And compared to embodiment one, the ketone content of organics in the present embodiment substantially increases
Plus.
<Example IV>
Step one, takes city organic sludge, and hydrothermal pretreatment is carried out at 300 DEG C, is generated after regathering hydrothermal pretreatment
Black liquor.
Step 2, by step one gained black liquor at -20 DEG C stored frozen 48 hours.
Step 3, prepares Zr (15.8)-FeOXCatalyst:By FeCl3Solution and ZrOCl2·8H2O solution pours into same appearance
Stirred in device, mixing time is 0.5~120min, is then filtrated to get Zr (15.8)-FeOXCatalyst.
Step 4, by Zr (the 15.8)-FeO obtained by step 3XCatalyst uses steam treatment 1h at 600 DEG C.
Step 5, by Zr (the 15.8)-FeO obtained by step 4XCatalyst is made under conditions of without any adhesive
Grain, crush and sieve, obtain Zr (15.8)-FeO that particle diameter is 300~850mmXCatalyst granules.
Step 6, takes the black liquor of stored frozen in 3.2g step 2, measurement obtains the content of wherein ketone organic matter
It is 14.97mg/mL.Take Zr (the 15.8)-FeO obtained by 0.2g step 5XThe particle of catalyst.By 3.2g black liquors and 0.2g
Zr(15.8)-FeOXThe particle of catalyst is added in reactor, and being passed through nitrogen makes the pressure of reactor reach 2MPa.
Step 7,250 DEG C are heated to by reactor.
Step 8, the agitating device in reactor is opened, and reacts 2h.
Step 9, the liquid substance after reaction terminates is collected by filter, obtains ketone organic matter, and measurement obtains it and contains
Amount 21.71mg/mL.
From the foregoing, the ketone measured in the ketone content of organics measured in sample after reaction and the preceding sample of reaction has
Machine thing content is compared, and increased 45%.And compared to embodiment one, the ketone content of organics in the present embodiment substantially increases
Plus.
<Embodiment five>
Step one, takes city organic sludge, and hydrothermal pretreatment is carried out at 300 DEG C, is generated after regathering hydrothermal pretreatment
Black liquor.
Step 2, by step one gained black liquor at -20 DEG C stored frozen 48 hours.
Step 3, prepares Zr (7.7)-FeOXCatalyst:By FeCl3Solution and ZrOCl2·8H2O solution pours into same appearance
Stirred in device, mixing time is 0.5~120min, is then filtrated to get Zr (7.7)-FeOXCatalyst.
Step 4, by Zr (the 7.7)-FeO obtained by step 3XCatalyst uses steam treatment 1h at 600 DEG C.
Step 5, by Zr (the 7.7)-FeO obtained by step 4XCatalyst is made under conditions of without any adhesive
Grain, crush and sieve, obtain particle diameter for Zr (7.7)-FeOXCatalyst granules.
Step 6, takes the black liquor of stored frozen in 3.2g step 2, and measurement obtains the content of wherein ketone organic matter
It is 15.17mg/mL.Take Zr (the 7.7)-FeO obtained by 0.2g step 5XThe particle of catalyst.By 3.2g black liquors and 0.2g
Zr(7.7)-FeOXThe particle of catalyst is added in reactor, and being passed through nitrogen makes the pressure of reactor reach 2MPa.
Step 7,350 DEG C are heated to by reactor.
Step 8, the agitating device in reactor is opened, and reacts 2h.
Step 9, the liquid substance after reaction terminates is collected by filter, obtains ketone organic matter, and measurement obtains it and contains
Amount 21.69mg/mL.
From the foregoing, the ketone measured in the ketone content of organics measured in sample after reaction and the preceding sample of reaction has
Machine thing content is compared, and increased 43%.And compared to embodiment one, the ketone content of organics in the present embodiment substantially increases
Plus.
<Embodiment six>
Step one, takes city organic sludge, and hydrothermal pretreatment is carried out at 300 DEG C, is generated after regathering hydrothermal pretreatment
Black liquor.
Step 2, by step one gained black liquor at -20 DEG C stored frozen 48 hours.
Step 3, prepares Zr (7.7)-FeOXCatalyst:By FeCl3Solution and ZrOCl2·8H2O solution pours into same appearance
Stirred in device, mixing time is 0.5~120min, is then filtrated to get Zr (7.7)-FeOXCatalyst.
Step 4, by Zr (the 7.7)-FeO obtained by step 3XCatalyst uses steam treatment 1h at 600 DEG C.
Step 5, by Zr (the 7.7)-FeO obtained by step 4XCatalyst is made under conditions of without any adhesive
Grain, crush and sieve, obtain Zr (7.7)-FeO that particle diameter is 300~850mmXCatalyst granules.
Step 6, takes the black liquor of stored frozen in 3.2g step 2, measurement obtains the content of wherein ketone organic matter
It is 14.73mg/mL.Take Zr (the 7.7)-FeO obtained by 0.2g step 5XThe particle of catalyst.By 3.2g black liquors and 0.2g
Zr(7.7)-FeOXThe particle of catalyst is added in reactor, and being passed through nitrogen makes the pressure of reactor reach 2MPa.
Step 7,250 DEG C are heated to by reactor.
Step 8, the agitating device in reactor is opened, and reacts 4h.
Step 9, the liquid substance after reaction terminates is collected by filter, obtains ketone organic matter, and measurement obtains it and contains
Amount 22.98mg/mL.
From the foregoing, the ketone measured in the ketone content of organics measured in sample after reaction and the preceding sample of reaction has
Machine thing content is compared, and increased 56%.And compared to embodiment one, the ketone content of organics in the present embodiment substantially increases
Plus.
The effect of embodiment and effect
The method of the city organic sludge catalytic production ketone organic matter involved by above-described embodiment, by city organic sludge
By hydrothermal pretreatment, then reacted by adding catalyst, it is hereby achieved that the ketone organic matter with high added value.
As can be seen that embodiment two to embodiment six with the addition of granular Zr (Y)-FeO from above-described embodimentXCatalyst, compares
In the embodiment one for being not added with any catalyst, the yield of its ketone organic matter is dramatically increased, and uses the ketone being collected into
Organic matter is also more suitable for the practical application in production compared to directly more facilitating using the ketone organic matter in raw sewage.
The method of the city organic sludge catalytic production ketone organic matter in above-described embodiment have technological process it is short, production
Condition is simple, recycle sludge in have high added value ketone organic matter yield it is high the features such as, preferably solve tradition
The problems such as mode pollutes environment, valuable substance yield less, is especially suitable for industrial application.
Above-mentioned implementation method is the preferred case of the present embodiment, is not intended to limit the protection domain of the present embodiment.
Claims (9)
1. a kind of method of city organic sludge catalytic production ketone organic matter, it is characterised in that comprise the following steps:
Step one, takes city organic sludge, and hydrothermal pretreatment is carried out at 200~400 DEG C, after regathering the hydrothermal pretreatment
The black liquor of generation;
Step 2, stored frozen at least 24 hours at the black liquor of gained in step one is placed on into -20~0 DEG C;
Step 3, prepares Zr (Y)-FeOXCatalyst:By FeCl3Solution and ZrOCl2·8H2O solution is poured into same container fully
Stirring, is then filtrated to get the Zr (Y)-FeOXCatalyst, in Zr (Y)-FeOXIn, Y is load ZrO2Mass fraction,
FeOXRepresent the oxide of iron;
Step 4, by the Zr (the Y)-FeO obtained by step 3XCatalyst uses steam treatment at 500~800 DEG C;
Step 5, by the Zr (the Y)-FeO obtained by step 4XCatalyst is granulated under conditions of without any adhesive, pressed
It is broken and sieve, obtain the Zr (Y)-FeOXThe particle of catalyst;
Step 6, by the Zr (the Y)-FeO obtained by 0~1g step 5XStorage is freezed in the particle and 1~5g step 2 of catalyst
The black liquor deposited is added in reactor, and being passed through nitrogen makes the pressure of the reactor reach 0~10MPa;
Step 7,100~400 DEG C are heated to by reactor;
Step 8, the agitating device in the reactor is opened, and reacts 0~4h;
Step 9, the liquid substance after reaction terminates is collected by filter, obtains ketone organic matter.
2. the method for city organic sludge catalytic production ketone organic matter according to claim 1, it is characterised in that:
Wherein, in step one, the temperature of the hydrothermal pretreatment is 300 DEG C.
3. the method for city organic sludge catalytic production ketone organic matter according to claim 1, it is characterised in that:
Wherein, in step 2, the temperature of the stored frozen is -20 DEG C.
4. the method for city organic sludge catalytic production ketone organic matter according to claim 1, it is characterised in that:
Wherein, in step 3, mixing time is 0.5~120min.
5. the method for city organic sludge catalytic production ketone organic matter according to claim 1, it is characterised in that:
Wherein, in step 4, the temperature of the steam treatment is 600 DEG C, and process time is 0~2h.
6. the method for city organic sludge catalytic production ketone organic matter according to claim 1, it is characterised in that:
Wherein, in step 5, screening obtains the Zr (Y)-FeOXThe grain diameter of catalyst is 300~850mm.
7. the method for city organic sludge catalytic production ketone organic matter according to claim 1, it is characterised in that:
Wherein, in step 6, being passed through nitrogen makes the pressure of the reactor reach 2MPa.
8. the method for city organic sludge catalytic production ketone organic matter according to claim 1, it is characterised in that:
Wherein, in step 7, the heating-up temperature of the reactor is 250 DEG C.
9. the method for city organic sludge catalytic production ketone organic matter according to claim 1, it is characterised in that:
Wherein, in step 8, the reaction time is 2h.
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Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN104379754A (en) * | 2012-02-28 | 2015-02-25 | 特瑞克斯有限合伙公司 | Treatment of biomass |
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2017
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Patent Citations (1)
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CN104379754A (en) * | 2012-02-28 | 2015-02-25 | 特瑞克斯有限合伙公司 | Treatment of biomass |
Non-Patent Citations (1)
Title |
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ERI FUMOTO等: "Production of ketones from sewage sludge over zirconia-supporting iron oxide catalysts in a steam atmosphere", 《APPLIED CATALYSIS B: ENVIRONMENTAL》 * |
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