CN108147413A - It is a kind of with charcoal and discarded system with molecular sieve for preparing for the method for group's indigo plant pigment - Google Patents
It is a kind of with charcoal and discarded system with molecular sieve for preparing for the method for group's indigo plant pigment Download PDFInfo
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- CN108147413A CN108147413A CN201810006199.7A CN201810006199A CN108147413A CN 108147413 A CN108147413 A CN 108147413A CN 201810006199 A CN201810006199 A CN 201810006199A CN 108147413 A CN108147413 A CN 108147413A
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- indigo plant
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- charcoal
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
It is a kind of with charcoal and discarded system with molecular sieve for preparing for the method for group's indigo plant pigment, be related to a kind of method for preparing pigment, the present invention is main Material synthesis group indigo plant pigment using charcoal prepared by the abandoned biomass such as waste catalyst carrier molecule sieve and stalk.By raw material drying, ground and mixed is uniform, is placed in ceramic crucible, is compacted, sealing；The crucible being sealed is placed in progress temperature programming calcining in Muffle furnace, obtains group's indigo plant crude pigment product；Then group's indigo plant crude pigment product is subjected to pigmentation processing, then group's crude pigment product after washing is added in the sodium sulfite solution of heat and is stirred, finally washed, filter repeatedly again, is dry, crushing, obtaining product.Prepared group's indigo plant pigment is nontoxic, has the characteristics that high temperature resistant, light resistance, water resistance, alkali resistance, weatherability and non-secondary pollution.Bright color, yield is high, and product is stablized, simple production process, green economy environmental protection.
Description
Technical field
The present invention relates to inorganic pigment preparation methods, and in particular to a kind of to use charcoal and discarded system with molecular sieve for preparing for group's indigo plant face
The method of material.
Background technology
Group's indigo plant is a kind of inorganic pigment product, and chemical constitution is alumino-silicate, is a kind of artificial lapis lazuli pigment.Group
Blue pigment asepsis environment-protecting, not soluble in water, heat-resisting, light shine, high temperature resistant（500 below C are colour-fast）, strong coloring force, it is and weather-proof
Property, alkali resistance it is good, have excellent dispersibility.Since group has the effects that propose white, toning, coloring, in plastics, coating, conjunction
There is application into a variety of industries such as resin, printing ink, rubber, building, paper, detergent, drawing pigment.Possessed by it
Red phase blue cannot be reached by mixing other pigment, and only itself just has this characteristic.
At present, industrial productive group indigo plant adds in the raw materials such as sodium carbonate and sulphur, high-temperature calcination using kaolin as primary raw material
Obtained product, existing main problem is that raw material resources are limited, of high cost, so the yield of the group in China is small at present, greatly
Amount is by import.
With the fast development of petrochemical industry, a large amount of molecular sieve catalyst is used in petrochemical industry production, molecule
Sieve catalyst is failed after a number of uses as solid waste, is largely arbitrarily piled up, and is occupied cultivated land, contaminated soil, water source.Point
The composition of son sieve mainly based on silicon, aluminium, secondly sulphur, calcium, sodium, titanium, phosphorus, iron, etc. elements.The blue lattice of group is by silicon, aluminium
What the netted typical tetrahedral structure that oxide is formed was formed, sodium, sulphion are dispersed between lattice, is a kind of sodium aluminium of complexity
Thiosilicic acid salt.Characteristic based on molecular sieve can be as a kind of raw material of composite group.
Usually used activated carbon, charcoal or rosin etc. are reducing agent in the blue preparation process of group.China's biomass energy is suitable
It is abundant, only all kinds of agricultural wastes（Such as stalk）Stock number be equivalent to 3.08 hundred million tons of standard coals every year, such as
This part resource of fruit is utilized well, and people, which are equivalent to, to be gathered around there are one inexhaustible resource treasure-house.This biology
Matter has the features such as certain toughness, porosity, low-density, is a kind of recycling resource of amount bargain sale.Utilize biomass system
The reducing agent that standby charcoal is used as all living creatures's production can substantially reduce production cost.
Invention content
The object of the present invention is to provide it is a kind of with charcoal and discarded system with molecular sieve for preparing for the method for group's indigo plant pigment, this method is
A kind of application process of economic and environment-friendly multipurpose biomass carbon and discarded molecular sieve in no group of planes indigo plant pigment technology of preparing, it is raw
Production. art is simple, and reaction condition is mild, low energy consumption, green economy environmental protection.
It is a kind of with charcoal and discarded system with molecular sieve for preparing for the method for group's indigo plant pigment, step is as follows：
（1）Biomass is screened, and charcoal is prepared after processing；
（2）It is spare after discarded molecular sieve pretreatment；
（3）Processing is dried in discarded molecular sieve, sodium carbonate, elemental sulfur, charcoal；
（4）Raw material is ground, weigh, is uniformly mixed, is placed in ceramic crucible, is compacted, seals；
（5）Crucible is positioned over progress temperature programming calcining in Muffle furnace；
（6）Group's indigo plant crude pigment product will be prepared to be washed repeatedly with hot water, the crude product after washing is then then added to sodium sulfite
Agitator treating in hot water, then wash, dry, pulverization process.
Step（1）In biomass used can be one or more of maize straw, broomcorn straw, rice husk, sawdust etc.；
Step（2）In charcoal used be the reducing agent for preparing group's indigo plant pigment, and as the framework ingredient of pigment；
Step（2）In molecular sieve used be petrochemical industry production in waste catalyst carrier.
Step（3）Described in molecular sieve and the mass ratio of sodium carbonate be：1:1.25~4
Step（3）Described in molecular sieve and the mass ratio of elemental sulfur be：1:0.2~5
Step（3）Described in molecular sieve and biomass carbon mass ratio:1:0.02~8
Step（5）Described in first stage calcining the C of temperature room temperature~600, soaking time 30~90 minutes.
Step（5）Described in second stage calcining 600~800 C of temperature, soaking time 60~180 minutes.
Step（6）Described in sodium sulfite solution concentration 1~8%.
Step（6）Described in group's indigo plant crude pigment product and sodium sulfite solution solid-liquid mass ratio be 1:2~5.
Step（6）Described in the bath temperature of hot water be 40~100 C.
Step（6）Described in sodium sulfite solution 40~100 C of temperature.
A kind of multipurpose biomass carbon of the present invention and discarded system with molecular sieve for preparing are for the method for group's indigo plant pigment, specific steps
It is as follows：
（1）The screening of biomass, it is cleaned, is dried, crush after prepare charcoal；
（2）After discarded molecular sieve pretreatment, 200 C dehydration and drying 2h；
（3）By sodium carbonate, elemental sulfur, prepare charcoal baking oven under 110 C drying and dehydrating 2h；
（4）Raw material is ground, is weighed, uniformly mixing in proportion, is placed in ceramic crucible, is compacted, seals；
（5）Crucible is placed in Muffle furnace and carries out temperature programmed control setting calcining；
（6）Group's indigo plant crude pigment product of preparation with hot water is washed repeatedly, removes water soluble salt, then adds in the crude product after washing
Into the aqueous solution of 1%~8% sodium sulfite heat（Solid-to-liquid ratio is 1:2~5）Agitator treating stirs 5~10min, then wash,
Dry, pulverization process.
The advantage of the invention is that：
1. this method substitutes the traditional raw materials such as kaolin come composite group using the discarded molecular sieve with tetrahedral structural unit
Indigo plant makes a large amount of industrial waste molecular sieve recycling, realizes open pit mining.
2. the charcoal that this method also uses the preparation of agriculture waste biomass is raw material.The biomass carbon is in group's indigo plant pigment
Both reducing agent can be can function as in preparation process as a kind of primary raw material in group's indigo plant pigment.
3. making full use of the annual a large amount of biomass castoff agriculturally generated, it is allowed to turn waste into wealth, has both saved money
Source, and ecological environment is protected, reduce the cost of pigment.
4. preparation method reaction condition is mild, reaction time is short, and the raw material used is cheap, and low energy consumption, and yield is high.Heavy metal
Pigment is just gradually replaced because of the toxic action of its own by nontoxic non-metallic pigments.The blue pigment asepsis environment-protecting of group, is a kind of
Economic and environment-friendly safe pigment.
Group's pigment prepared by the present invention passes through experiment test, can meet following pigment patience test index：
After water resistance, pigment and water contact, the dissolving to water resistant is non-discolouring.
Heat resistance, for pigment in 500 C, heat preservation 120h is colour-fast.
Alkali resistance, impregnate in 2% sodium hydrate aqueous solution 120 hours it is non-discolouring.
Light shine, it is colour-fast in ultra violet lamp 120h.
Solvent resistance, pigment and solvent contact position are colour-fast to the dissolving of anti-solvent.
Description of the drawings
Fig. 1 is the product figure of group's indigo plant pigment prepared by embodiment 1；
Fig. 2 is the XRD spectrum of group's indigo plant pigment prepared by embodiment 1；
Fig. 3 is the infared spectrum of group's indigo plant pigment prepared by embodiment 1.
Specific embodiment
The present invention presented below is using a kind of biomass carbon and discarded system with molecular sieve for preparing for the specific implementation method of group's indigo plant pigment：
Embodiment 1
Biomass is fired into biomass carbon, 80 C are first risen to from room temperature with the speed of 5 C/min under the atmosphere of nitrogen, then from
80 C are warming up to 300 C with the speed of 10 C/min, keep the temperature 30min, and Temperature fall is spare by the charcoal being fired into.It will
Na2CO3 , elemental sulfur, biomass carbon dry 2 hours under 110 C, discard molecular sieve and dried 2 hours in 200 C；Weigh molecule
2000 gram molecules sieve is sieved, 1000 grams of elemental sulfur, 1500 grams of sodium carbonate, 1000 grams of biomass carbon is ground, uniformly mixed, is placed in pottery
It in porcelain crucible, is compacted, sealing.Ceramic crucible is placed in Muffle furnace, rising to 500 C with the speed of 10 C/min carries out the first rank
Section calcining, using temperature programming, constant temperature 50 minutes continues to heat up, and carrying out second stage with the speed of 10 C/min to 600 C forges
It burns, constant temperature 60 minutes obtains group's indigo plant crude product.Crude product carries out pigmentation processing, by the crude product of preparation in 40 C hot water
It washs repeatedly, removes water soluble salt, group's crude pigment product after washing is in 2%, 80 C sodium sulfite solutions（Solid-to-liquid ratio is
1:2）Stir 5min, then wash, dry, crushing, being sieved obtains group's indigo plant pigment of pure uniform particle sizes.
Embodiment 2
Biomass is fired into biomass carbon, 150 C are first risen to from room temperature with the speed of 8 C/min under the atmosphere of nitrogen, then
400 C are warming up to from 150 C with the speed of 15 C/min, keep the temperature 60min, Temperature fall is spare by the charcoal being fired into.It will
Na2CO3, elemental sulfur, biomass carbon dry 2 hours under 110 C, discard molecular sieve and dried 2 hours in 200 C；Weigh molecular sieve
2000 gram molecules sieve, 1500 grams of elemental sulfur, 4000 grams of sodium carbonate, 2000 grams of biomass carbon, grind, and are uniformly mixed, are placed in ceramics
It in crucible, is compacted, sealing.Ceramic crucible is placed in Muffle furnace, rising to 600 C with the speed of 5 C/min carries out the first stage
Calcining, using temperature programming, constant temperature 40 minutes continues to heat up, and rising to 700 C progress second stage with the speed of 5 C/min forges
It burns, constant temperature 80 minutes obtains group's indigo plant crude product.Crude product carries out pigmentation processing, and the crude product of preparation is washed repeatedly in 70 C hot water
It washs, removes water soluble salt, group's crude pigment product after washing is in 3%, 80 C sodium sulfite solutions（Solid-to-liquid ratio is 1:3）Stirring
10min, then wash, dry, crushing, being sieved obtains group's indigo plant pigment of pure uniform particle sizes.
Embodiment 3
Biomass is fired into biomass carbon, 100 C are first risen to from room temperature with the speed of 10 C/min under the atmosphere of nitrogen, then
200 C are warming up to from 100 C with the speed of 5 C/min, keep the temperature 80min, Temperature fall is spare by the charcoal being fired into.It will
Na2CO3 , elemental sulfur, biomass carbon dry 2 hours under 110 C, discard molecular sieve and dried 2 hours in 200 C；Weigh molecule
2000 grams of sieve, 3000 grams of elemental sulfur, 1500 grams of sodium carbonate, 3000 grams of biomass carbon are ground, and are uniformly mixed, are placed in ceramic crucible
In, it is compacted, sealing.Ceramic crucible is placed in Muffle furnace, with the speed of 15 C/min rise to 700 C carry out the first stage forge
It burns, using temperature programming, constant temperature 60 minutes, 350 C of cooling carry out second stage calcining, and constant temperature 70 minutes obtains group's indigo plant crude product.
Crude product carries out pigmentation processing, and the crude product of preparation is washed repeatedly in 60 C hot water, removes water soluble salt, group's face after washing
Expect crude product in 4%, 70 C sodium sulfite solutions（Solid-to-liquid ratio is 1:4）8min is stirred, then washes, dry, crush, be sieved
To group's indigo plant pigment of pure uniform particle sizes.
Embodiment 4
Biomass is fired into biomass carbon, 200 C are first risen to from room temperature with the speed of 5 C/min under the atmosphere of nitrogen, then
400 C are warming up to from 200 C with the speed of 5 C/min, keep the temperature 90min, Temperature fall will
The charcoal being fired into is spare.By Na2CO3 , elemental sulfur, biomass carbon dry 2 hours under 110 C, discard molecular sieve
It is dried 2 hours in 200 C；Weigh 2000 grams of molecular sieve, 2000 grams of elemental sulfur, 6000 grams of sodium carbonate, 2000 grams of biomass carbon grinds
Mill is uniformly mixed, is placed in ceramic crucible, is compacted, sealing.Ceramic crucible is placed in Muffle furnace, with the speed liter of 5 C/min
First stage calcining is carried out to 700 C, using temperature programming, constant temperature 40 minutes is continued to heat up, be risen to the speed of 5 C/min
800 C carry out second stage calcining, and constant temperature 90 minutes obtains group's indigo plant crude product.Crude product carries out pigmentation processing, by the crude product of preparation
It is washed repeatedly in 60 C hot water, removes water soluble salt, group's indigo plant crude pigment product after washing is in 5%, 90 C sodium sulfite solutions
In（Solid-to-liquid ratio is 1:5）6min is stirred, then washes, dry, crush, obtains group's indigo plant pigment of pure uniform particle sizes.
Embodiment 5
Biomass is fired into biomass carbon, 150 C are first risen to from room temperature with the speed of 15 C/min under the atmosphere of nitrogen, then
450 C are warming up to from 150 C with the speed of 5 C/min, keep the temperature 100min, Temperature fall is spare by the charcoal being fired into.It will
Na2CO3 , elemental sulfur, biomass carbon dry 2 hours under 110 C, discard molecular sieve and dried 2 hours in 200 C；Weigh molecule
2000 grams of sieve, 4000 grams of elemental sulfur, 2500 grams of sodium carbonate, 3000 grams of biomass carbon are ground, and are uniformly mixed, are placed in ceramic crucible
In, it is compacted, sealing.Ceramic crucible is placed in Muffle furnace, rising to 650 C with the speed of 5 C/min carries out first stage calcining,
Using temperature programming, constant temperature 50 minutes, Temperature fall, until 450 C carry out second stage calcining, constant temperature 30 minutes obtains group's indigo plant
Crude product.Crude product carries out pigmentation processing, and the crude product of preparation is washed repeatedly in 100 C hot water, water soluble salt is removed, after washing
Group's crude pigment product in 2%, 80 C sodium sulfite solutions（Solid-to-liquid ratio is 1:2）7min is stirred, then wash, dry, crushing,
Sieving obtains group's indigo plant pigment of pure uniform particle sizes.
Embodiment 6
Biomass is fired into biomass carbon, 200 C are first risen to from room temperature with the speed of 10 C/min under the atmosphere of nitrogen, then
550 C are warming up to from 200 C with the speed of 10 C/min, keep the temperature 150min, Temperature fall is spare by the charcoal being fired into.It will
Na2CO3 , elemental sulfur, biomass carbon dry 2 hours under 110 C, discard molecular sieve and dried 2 hours in 200 C；Weigh 2000
Gram, 3000 grams of elemental sulfur, 1500 grams of sodium carbonate, 1000 grams of biomass carbon is ground, uniformly mixed, is placed in ceramic crucible, is pressed
It is real, sealing.Ceramic crucible is placed in Muffle furnace, rising to 500 C with the speed of 15 C/min carries out first stage calcining, uses
Temperature programming, constant temperature 30 minutes, continues to heat up, and rising to 750 C with the speed of 15 C/min carries out second stage calcining, constant temperature 60
Minute, obtain group's indigo plant crude product.Crude product carries out pigmentation processing, and the crude product of preparation is anti-in 70 C hot water
After backwashing is washed, and removes water soluble salt, group's crude pigment product after washing is in 3%, 100 C sodium sulfite solutions
（Solid-to-liquid ratio is 1:3）Stir 9min, then wash, dry, crushing, being sieved obtains group's indigo plant pigment of pure uniform particle sizes.
Claims (6)
1. it is a kind of with charcoal and discarded system with molecular sieve for preparing for the method for group's indigo plant pigment, which is characterized in that the method step is：
（1）Screening, processing and the preparation of charcoal of biomass；Charcoal is prepared as：The biomass for weighing pretreatment is placed in
In tube furnace；Nitrogen is passed through in quartz ampoule, air is emptied；The lower temperature programming of nitrogen protection：Room temperature~200 C, 10~90
min；200~600 C, 30~120 min；30~180 min are kept the temperature, then Temperature fall；
（2）It is spare after discarded molecular sieve pretreatment；
（3）Processing is dried in discarded molecular sieve, sodium carbonate, elemental sulfur, charcoal；
（4）Raw material is ground, is weighed, uniformly mixing, raw material proportioning are in proportion：The mass ratio of molecular sieve and sodium carbonate is
1:1.25~4；The mass ratio of molecular sieve and elemental sulfur is 1:0.2~5；The mass ratio 1 of molecular sieve and charcoal:0.02~8；It puts
In ceramic crucible, compacting seals；
（5）Crucible is placed in progress temperature programmed control calcining in Muffle furnace；Calcining heating mode is：The C of first stage room temperature~600,
Time is 30~90min；600~800 C of second stage, time are 60~180min；
（6）Group's indigo plant crude pigment product of preparation with hot water is washed repeatedly, the crude product after washing is then added to sodium sulfite heat
Agitator treating in water, then wash, dry, crushing, be sieved processing to get.
2. according to claim 1 it is a kind of with charcoal and discarded system with molecular sieve for preparing for the method for group's indigo plant pigment, which is characterized in that
Step（1）Biomass used is one or more of maize straw, broomcorn straw, rice husk, sawdust.
3. according to claim 1 it is a kind of with charcoal and discarded system with molecular sieve for preparing for the method for group's indigo plant pigment, which is characterized in that
Step（3）Charcoal used is the reducing agent for preparing group's indigo plant pigment, and as the framework ingredient of pigment.
4. according to claim 1 it is a kind of with charcoal and discarded system with molecular sieve for preparing for the method for group's indigo plant pigment, which is characterized in that
Step（3）In molecular sieve used be petrochemical industry production in waste catalyst carrier.
5. according to claim 1 it is a kind of with charcoal and discarded system with molecular sieve for preparing for the method for group's indigo plant pigment, which is characterized in that
Step（6）Described in group's indigo plant crude pigment product and sodium sulfite solution mass ratio（Solid-to-liquid ratio）It is 1:2~5.
6. according to claim 1 it is a kind of with charcoal and discarded system with molecular sieve for preparing for the method for group's indigo plant pigment, which is characterized in that
Step（6）Described in sodium sulfite solution a concentration of 1-8%.
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| CN201810006199.7A CN108147413A (en) | 2018-01-04 | 2018-01-04 | It is a kind of with charcoal and discarded system with molecular sieve for preparing for the method for group's indigo plant pigment |
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| CN201810006199.7A CN108147413A (en) | 2018-01-04 | 2018-01-04 | It is a kind of with charcoal and discarded system with molecular sieve for preparing for the method for group's indigo plant pigment |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110330024A (en) * | 2019-04-03 | 2019-10-15 | 沈阳化工大学 | A method of ultramarine green pigment is prepared with discarded molecular sieve and charcoal |
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| CN104059394A (en) * | 2014-07-08 | 2014-09-24 | 山东慧科助剂股份有限公司 | Method for preparing ultramarine blue pigment |
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2018
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104059394A (en) * | 2014-07-08 | 2014-09-24 | 山东慧科助剂股份有限公司 | Method for preparing ultramarine blue pigment |
Non-Patent Citations (2)
| Title |
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| 初政伟等: "废弃分子筛制备群蓝颜料研究", 《广工化工》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110330024A (en) * | 2019-04-03 | 2019-10-15 | 沈阳化工大学 | A method of ultramarine green pigment is prepared with discarded molecular sieve and charcoal |
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Application publication date: 20180612 |