CN107376861A - A kind of preparation method of recyclability deoxidier - Google Patents
A kind of preparation method of recyclability deoxidier Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- 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
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- 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
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Abstract
The invention discloses a kind of preparation method of recyclability deoxidier, belong to deoxidier technical field.The present invention is using iron powder as base-material, diatomite and activated carbon are carrier, first iron oxide is reduced, reduced iron powder and diatomite, salt and Grape Skin blending are fermented, reduced iron powder, salt and diatom generation free state mixture, the oxygen uptake performance of metallic element is set to improve the deoxidation effect of activated carbon using microorganism.Liquid feeding body whipping cream, compatibility is improved, continuously adds alkaline earth oxide, improve the content of reduced iron powder, then its internal void space is become big with montmorillonite, improve its deoxidation capacity.Finally, liquefied mixture with deoxygenation function is coated in carrier surface, deoxidier is made, the use of deoxidier, outermost layer saturation come off, and expose new deoxidation composition, extend deoxidier regeneration cycle, reduce energy expenditure, significantly improve the regenerability and deoxidation capacity of deoxidier, have broad application prospects.
Description
Technical field belongs to deoxidier technical field the invention discloses a kind of preparation method of recyclability deoxidier.
Background technology
The research of domestic deoxidier starts from 20th century the fifties end, and it is that deoxidation is urged that Nan Hua companies, which start production 0603 the sixties,
Agent.0603 system is using the oxide of copper as key component, and it both can be in H2In the presence of deoxidation, can also be under hydrogen-free condition
Deoxidation, deoxidation depth are 1.0 × 10-5, deoxidizing capacity 10ml/g.0605 after improvement improves deoxy activity and machinery
Intensity, depth are 5.0 × 10-6.The said firm in 1984 releases BH series dehydrogenation catalysts again, and BH series is using Ni as activearm
Point, can both there is H2Under conditions of deoxidation, chemical absorbing deoxidation can also be made, can be by general nitrogen, argon gas and hydro carbons mixing qi exhaustion
To 5.0 × 10-6, deoxidizing capacity is up to 25ml/g.
The DO series deoxidiers that the Lanzhou Chemistry and Physics Institute of the Chinese Academy of Sciences develops are using Pt, Pa as active component, for synthetic gas deoxidizing.
Because its preparation method is to use infusion process, thin-shell type bimetallic or single-metal reforming catalyst is made, so efficiency is higher, deoxy activity
Height, stability is good, and side reaction is few；It is but undesirable when CO is high in raw material.The Dalian Chemistry and Physics Institute of the Chinese Academy of Sciences develops a kind of palladium/manganese oxide
Deoxidier, its principle are that the oxide of low price manganese has high activity to micro amount of oxygen, can react generation value Mn at normal temperatures
With reaching deoxidation mesh, the oxide hydrogen reduction of value Mn has recovered deoxy activity, led to oxide again into the oxide of low price manganese
Cross deoxidation and regeneration, remove the water of generation, so as to reach deoxidier it is long-term, stably, efficient deoxy performance.
With industrial expansion, the requirement to high-purity gas improves constantly from quality and quantity, the requirement to deoxidier
Also accordingly increasing, especially recyclability deoxidier.So the new renewable deoxidier of exploitation is by before with wide market
Scape.
The content of the invention
The technical problems to be solved by the invention：Have that regeneration rate is relatively low low with deoxidation capacity to be lacked for current deoxidier
Fall into, there is provided a kind of preparation method of recyclability deoxidier.
In order to solve the above-mentioned technical problem, the present invention is using technical scheme as described below：
A kind of preparation method of recyclability deoxidier, it is characterised in that specifically preparation process is：
（1）80~100g steels are weighed, after grating into strips, strip-like-shaped steel is obtained, strip-like-shaped steel is put into roaster
Aoxidized, iron oxide is obtained after oxidation, continue iron oxide being put into roaster, the reduction reaction under nitrogen guard mode,
Reduced iron powder is obtained after reduction；
（2）The grinding of 4~6g diatomite is weighed again, and diatomite powder is obtained after grinding；
（3）Reduced iron powder, salt and diatomite powder are mixed, mixture is obtained after stirring, continues to add into mixture
Enter the Grape Skin of mixture quality 0.6%, be fitted into fermentation tank, be sealed by fermentation, after fermentation ends, take out tunning, as swim
Amorph mixture；
（4）Added again into free state mixture 3~5g activated carbons, 100~200mL fresh liquid milks oil, 2~4g calcium oxide and
800~1000mL water is mixed, and liquefied mixture is obtained after stirring；
（5）Take montmorillonite to be taken out after being soaked in water, freeze 3~5min with liquid nitrogen spraying immediately, after its clear-cutting forestland room temperature, obtain
To pretreatment montmorillonite；By liquefied mixture with hairbrush coated in montmorillonite surface is pre-processed, it is 2~5mm to control coating thickness,
After coating terminates, deoxidier base substrate is obtained；
（6）Deoxidier base substrate is put into baking oven, is transferred in Muffle furnace after being dried at 105~110 DEG C, is burnt at 300~400 DEG C
Knot, produces recyclability deoxidier after discharging.
Step（1）The oxidizing temperature of described roaster is 950~1000 DEG C, and the reduction temperature of roaster is 800~900
DEG C, oxidization time is 2~3h, and the recovery time is 1~2h.
Step（2）Described milling time is 6~9min.
Step（3）The mass ratio of described reduced iron powder, salt and diatomite powder is 5：1：2, mixing time be 7~
9min, fermentation temperature are 45~55 DEG C, and fermentation time is 7~9 days.
Step（4）Described mixing time is 10~30min.
Step（5）Described soak time is 1~2h.
Step（6）Described drying time is 1~2h, and sintering time is 1~2h.
The beneficial effects of the invention are as follows：
For the present invention using iron powder as base-material, diatomite and activated carbon are carrier, and iron oxide is reduced first, gone back after reduction
Former iron powder, reduced iron powder are easy to aoxidize, and reduced iron powder and diatomite, salt and Grape Skin blending are fermented, utilize microorganism pair
Reduced iron powder, salt and diatomite act and generate free state mixture, will be free under the self-crosslinking of microorganism
State mixture is incorporated into activated carbon surface, improves the deoxidation effect of activated carbon using the oxygen uptake performance of metallic element so that final
Obtained deoxidier has splendid oxygen uptake performance, adds fresh liquid milk oil, improves free state mixture and activated carbon
Compatibility, alkaline earth oxide is continuously added, considerably improve the content of active constituent reduced iron powder in deoxidier, then with
Montmorillonite splits principle using ice, deoxidier carrier inside interstitial space can be made to become big, taken off so as to improve it as deoxidation agent carrier
Oxygen capacity, finally, the liquefied mixture with deoxygenation function is coated in carrier surface, deoxidier is made, with deoxidier
Use, the deoxidation capacity that its outermost layer has the liquefied mixture of deoxygenation function can progressively reach saturation state and natural aging takes off
Fall, expose internal new deoxygenation function composition again, so as to reach regeneration purpose, extend deoxidier regeneration cycle, subtract
Energy expenditure is lacked, has significantly improved the regenerability and deoxidation capacity of deoxidier, have broad application prospects.
Embodiment
80~100g steels are weighed, after grating into strips, obtain strip-like-shaped steel, strip-like-shaped steel is put into temperature is
2~3h of oxidation is carried out in 950~1000 DEG C of roaster, iron oxide is obtained after oxidation, continues iron oxide being put into roaster,
It is 800~900 DEG C to set temperature, 1~2h of reduction reaction under nitrogen guard mode, reduced iron powder is obtained after reduction, then weigh 4
~6g diatomite grinds 6~9min, and diatomite powder is obtained after grinding, is in mass ratio 5：1：2 by reduced iron powder, salt and silicon
Diatomaceous earth powder mixes 7~9min, and mixture is obtained after stirring, continues to add mixture quality 0.6 into mixture
% Grape Skin, is fitted into fermentation tank, is sealed by fermentation 7~9 days under conditions of being 45~55 DEG C in temperature, after fermentation ends,
Tunning, as free state mixture are taken out, then 3~5g activated carbons, 100~200mL liquid are added into free state mixture
Body whipping cream, 2~4g calcium oxide and 800~1000mL water mix 10~30min, and liquefied mixture is obtained after stirring；Take
Montmorillonite is soaked in water after 1~2h and taken out, and freezes 3~5min with liquid nitrogen spraying immediately, after its clear-cutting forestland room temperature, obtains pre-
Montmorillonite is handled, by liquefied mixture with hairbrush coated in pretreatment montmorillonite surface, it is 2~5mm to control coating thickness, coating
After end, deoxidier base substrate is obtained, deoxidier base substrate is put into baking oven, Muffle is transferred to after drying 1~2h at 105~110 DEG C
In stove, 1~2h is sintered at 300~400 DEG C, recyclability deoxidier is produced after discharging.
Example 1 weighs 80g steels, after grating into strips, obtains strip-like-shaped steel, and strip-like-shaped steel is put into temperature is
Oxidation 2h is carried out in 950 DEG C of roaster, iron oxide is obtained after oxidation, continues iron oxide being put into roaster, temperature is set
For 800 DEG C, the reduction reaction 1h under nitrogen guard mode, reduced iron powder is obtained after reduction, then weighs 4g diatomite grinding 6min,
Diatomite powder is obtained after grinding, is in mass ratio 5：1：Reduced iron powder, salt and diatomite powder are mixed 7min by 2,
Mixture is obtained after stirring, continues to add the Grape Skin of mixture quality 0.6% into mixture, is fitted into fermentation tank, in temperature
To be sealed by fermentation 7 days under conditions of 45 DEG C, after fermentation ends, tunning, as free state mixture are taken out, then to free state
3g activated carbons, 100mL fresh liquid milks oil, 2g calcium oxide and 800mL water are added in mixture and mixes 10min, after stirring
To liquefied mixture；Take montmorillonite to be soaked in water after 1h to take out, freeze 3min with liquid nitrogen spraying immediately, treat its clear-cutting forestland room temperature
Afterwards, obtain pre-processing montmorillonite, by liquefied mixture with hairbrush coated in pretreatment montmorillonite surface, control the coating thickness to be
2mm, after coating terminates, deoxidier base substrate is obtained, deoxidier base substrate is put into baking oven, Muffle is transferred to after drying 1h at 105 DEG C
In stove, 1h is sintered at 300 DEG C, recyclability deoxidier is produced after discharging.
Example 2
90g steels are weighed, after grating into strips, obtain strip-like-shaped steel, strip-like-shaped steel is put into the roasting that temperature is 950 DEG C
Oxidation 2h is carried out in stove, iron oxide is obtained after oxidation, continues iron oxide being put into roaster, it is 850 DEG C to set temperature, in nitrogen
Reduction reaction 1h under gas shielded state, obtains reduced iron powder after reduction, then weighs 5g diatomite grinding 8min, and silicon is obtained after grinding
Diatomaceous earth powder, it is in mass ratio 5：1：Reduced iron powder, salt and diatomite powder are mixed 8min by 2, are mixed after stirring
Compound, continue to add the Grape Skin of mixture quality 0.6% into mixture, be fitted into fermentation tank, in the condition that temperature is 50 DEG C
It is lower to be sealed by fermentation 8 days, after fermentation ends, take out tunning, as free state mixture, then added into free state mixture
4g activated carbons, 150mL fresh liquid milks oil, 3g calcium oxide and 900mL water mix 20min, and liquefied mixture is obtained after stirring；
Take montmorillonite to be soaked in water after 1h to take out, freeze 4min with liquid nitrogen spraying immediately, after its clear-cutting forestland room temperature, pre-processed
Montmorillonite, by liquefied mixture with hairbrush coated in montmorillonite surface is pre-processed, it is 4mm to control coating thickness, after coating terminates,
Deoxidier base substrate is obtained, deoxidier base substrate is put into baking oven, is transferred in Muffle furnace after drying 1h at 105 DEG C, is burnt at 350 DEG C
1h is tied, recyclability deoxidier is produced after discharging.
Example 3
100g steels are weighed, after grating into strips, obtain strip-like-shaped steel, strip-like-shaped steel is put into the roasting that temperature is 1000 DEG C
Burn in stove and carry out oxidation 3h, obtain iron oxide after oxidation, continue iron oxide being put into roaster, it is 900 DEG C to set temperature,
Reduction reaction 2h under nitrogen guard mode, obtains reduced iron powder after reduction, then weighs 6g diatomite grinding 9min, is obtained after grinding
Diatomite powder, it is in mass ratio 5：1：Reduced iron powder, salt and diatomite powder are mixed 9min by 2, are obtained after stirring
Mixture, continue to add the Grape Skin of mixture quality 0.6% into mixture, be fitted into fermentation tank, in the bar that temperature is 55 DEG C
It is sealed by fermentation 9 days under part, after fermentation ends, takes out tunning, as free state mixture, then add into free state mixture
Enter 5g activated carbons, 200mL fresh liquid milks oil, 4g calcium oxide and 1000mL water and mix 30min, liquid mixing is obtained after stirring
Thing；Take montmorillonite to be soaked in water after 2h to take out, freeze 5min with liquid nitrogen spraying immediately, after its clear-cutting forestland room temperature, obtain pre-
Montmorillonite is handled, by liquefied mixture with hairbrush coated in pretreatment montmorillonite surface, it is 5mm to control coating thickness, coating knot
Shu Hou, deoxidier base substrate is obtained, deoxidier base substrate is put into baking oven, be transferred to after drying 2h at 110 DEG C in Muffle furnace, 400
2h is sintered at DEG C, recyclability deoxidier is produced after discharging.
The deoxidier that comparative example is produced with Guangzhou company takes off to recyclability produced by the present invention as a comparison case
Deoxidier in oxygen agent and comparative example is detected, and testing result is as shown in table 1：1st, method of testing
Deoxidation depth test is detected by the standard with deoxidation deep regenerative time experiment, and deoxidation depth is oxygen after gas deoxidation
The ratio of oxygen volume before volume and gas deoxidation；
And the deoxidation capacity of product is detected, deoxidation capacity refers to that unit mass deoxidier is capable of the oxygen volume of adsorbing and removing, tool
Body testing result is as shown in table 1：
Table 1
It can be seen from data in table 1, the deoxidizing capacity of recyclability deoxidier produced by the present invention is strong, and deoxidation capacity is high, and energy
It is enough voluntarily to regenerate, there is wide prospect of the application.
Claims (7)
1. a kind of preparation method of recyclability deoxidier, it is characterised in that specifically preparation process is：
（1）80~100g steels are weighed, after grating into strips, strip-like-shaped steel is obtained, strip-like-shaped steel is put into roaster
Aoxidized, iron oxide is obtained after oxidation, continue iron oxide being put into roaster, the reduction reaction under nitrogen guard mode,
Reduced iron powder is obtained after reduction；
（2）The grinding of 4~6g diatomite is weighed again, and diatomite powder is obtained after grinding；
（3）Reduced iron powder, salt and diatomite powder are mixed, mixture is obtained after stirring, continues to add into mixture
Enter the Grape Skin of mixture quality 0.6%, be fitted into fermentation tank, be sealed by fermentation, after fermentation ends, take out tunning, as swim
Amorph mixture；
（4）Added again into free state mixture 3~5g activated carbons, 100~200mL fresh liquid milks oil, 2~4g calcium oxide and
800~1000mL water is mixed, and liquefied mixture is obtained after stirring；
（5）Take montmorillonite to be taken out after being soaked in water, freeze 3~5min with liquid nitrogen spraying immediately, after its clear-cutting forestland room temperature, obtain
To pretreatment montmorillonite, by liquefied mixture with hairbrush coated in montmorillonite surface is pre-processed, it is 2~5mm to control coating thickness,
After coating terminates, deoxidier base substrate is obtained；
（6）Deoxidier base substrate is put into baking oven, is transferred in Muffle furnace after being dried at 105~110 DEG C, is burnt at 300~400 DEG C
Knot, produces recyclability deoxidier after discharging.
A kind of 2. preparation method of recyclability deoxidier according to claim 1, it is characterised in that：Step（1）It is described
The oxidizing temperature of roaster be 950~1000 DEG C, the reduction temperature of roaster is 800~900 DEG C, and oxidization time is 2~3h,
Recovery time is 1~2h.
A kind of 3. preparation method of recyclability deoxidier according to claim 1, it is characterised in that：Step（2）It is described
Milling time be 6~9min.
A kind of 4. preparation method of recyclability deoxidier according to claim 1, it is characterised in that：Step（3）It is described
Reduced iron powder, the mass ratio of salt and diatomite powder be 5：1：2, mixing time is 7~9min, fermentation temperature is 45~
55 DEG C, fermentation time is 7~9 days.
A kind of 5. preparation method of recyclability deoxidier according to claim 1, it is characterised in that：Step（4）It is described
Mixing time be 10~30min.
A kind of 6. preparation method of recyclability deoxidier according to claim 1, it is characterised in that：Step（5）It is described
Soak time be 1~2h.
A kind of 7. preparation method of recyclability deoxidier according to claim 1, it is characterised in that：Step（6）It is described
Drying time be 1~2h, sintering time is 1~2h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109294338A (en) * | 2018-08-31 | 2019-02-01 | 王成 | A kind of preparation method of metal protection deoxidier |
| CN111792926A (en) * | 2020-07-23 | 2020-10-20 | 李笑天 | Method for preparing embryo body by using rare earth element-iron oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103653185A (en) * | 2013-11-13 | 2014-03-26 | 广西弘耀祥科技有限公司 | Moisture-proof deoxidizing agent for foodstuff |
| CN105076389A (en) * | 2015-07-23 | 2015-11-25 | 小嵩保鲜技术(常熟)有限公司 | Deoxidizer and making method thereof |
| CN105995383A (en) * | 2016-06-16 | 2016-10-12 | 常熟市屹浩食品包装材料科技有限公司 | Rapid deoxidizer for foods and preparation method of deoxidizer |
| CN106977230A (en) * | 2017-05-14 | 2017-07-25 | 石磊 | A kind of preparation method of water conservation self-repair type curing compound |
-
2017
- 2017-08-30 CN CN201710763980.4A patent/CN107376861A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103653185A (en) * | 2013-11-13 | 2014-03-26 | 广西弘耀祥科技有限公司 | Moisture-proof deoxidizing agent for foodstuff |
| CN105076389A (en) * | 2015-07-23 | 2015-11-25 | 小嵩保鲜技术(常熟)有限公司 | Deoxidizer and making method thereof |
| CN105995383A (en) * | 2016-06-16 | 2016-10-12 | 常熟市屹浩食品包装材料科技有限公司 | Rapid deoxidizer for foods and preparation method of deoxidizer |
| CN106977230A (en) * | 2017-05-14 | 2017-07-25 | 石磊 | A kind of preparation method of water conservation self-repair type curing compound |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109294338A (en) * | 2018-08-31 | 2019-02-01 | 王成 | A kind of preparation method of metal protection deoxidier |
| CN109294338B (en) * | 2018-08-31 | 2021-01-19 | 上海集优张力控制螺栓有限公司 | Preparation method of metal protection deoxidizer |
| CN111792926A (en) * | 2020-07-23 | 2020-10-20 | 李笑天 | Method for preparing embryo body by using rare earth element-iron oxide |
| CN111792926B (en) * | 2020-07-23 | 2023-12-19 | 李笑天 | Method for preparing embryo body from rare earth element-iron oxide |
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