CN106592312B - The method for recycling slurrying yellow liquor solid base coproduction organic ammonium quick-acting fertilizer and slow-release fertilizer - Google Patents
The method for recycling slurrying yellow liquor solid base coproduction organic ammonium quick-acting fertilizer and slow-release fertilizer Download PDFInfo
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- CN106592312B CN106592312B CN201611190506.9A CN201611190506A CN106592312B CN 106592312 B CN106592312 B CN 106592312B CN 201611190506 A CN201611190506 A CN 201611190506A CN 106592312 B CN106592312 B CN 106592312B
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Classifications
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C11/00—Regeneration of pulp liquors or effluent waste waters
- D21C11/04—Regeneration of pulp liquors or effluent waste waters of alkali lye
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
- C01B25/451—Phosphates containing plural metal, or metal and ammonium containing metal and ammonium
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C11/00—Regeneration of pulp liquors or effluent waste waters
- D21C11/0007—Recovery of by-products, i.e. compounds other than those necessary for pulping, for multiple uses or not otherwise provided for
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Fertilizers (AREA)
Abstract
The method for recycling slurrying yellow liquor solid base coproduction organic ammonium quick-acting fertilizer and slow-release fertilizer, for fibre plant after solid base pulping process boiling, reaction product obtains paper pulp and slurrying yellow liquor through separation of solid and liquid；Slurrying yellow liquor is heated to reflux, bicarbonate is decomposed, solid content I and liquid I is obtained through separation of solid and liquid；Ammonium hydroxide is added in into liquid I, precipitation is generated, solid content II and filtrate II is obtained after separation of solid and liquid；Ammonium hydroxide is added in into liquid I to precipitation is no longer generated, solid content III and filtrate II I is obtained after separation of solid and liquid；By solid content I and solid content II or solid content III through cleaning, drying, roasting, solid base is recycled；It is 5~8 that phosphoric acid is added in into filtrate II or filtrate II I to pH, and solid content IV and filtrate IV is obtained after separation of solid and liquid；It is dried after solid content IV is washed to get slow-release fertilizer ammonium magnesium phosphate；Filtrate IV is used as compound liquid fertilizer or compound fertilizer that is concentrated, being granulated, lignin ammonium salt and ammonium phosphate salt are obtained after drying.
Description
Technical field
The present invention relates to chemical fertilizer, more particularly, to a kind of recycling slurrying yellow liquor solid base coproduction organic ammonium quick-acting fertilizer and
The method of slow-release fertilizer.
Background technology
In recent years, traditional paper industry is faced with the upgrading and transformation of industrial technology.Chinese patent CN101532260B is disclosed
A kind of brand-newpulping method of the cooking solid base of fibre plant, this method will accelerate cleaning pulping with preparing high level chemicals
Etc. biomass energies Chemical Engineering Technology industrialization.Chinese patent CN105332309A discloses a kind of same from solid base slurrying yellow liquor
The method of one-step separation of wood quality and recycling solid base, this method carry for the processing of solid base slurrying yellow liquor and the recycling of active ingredient
Good thinking is supplied, but it uses the remaining yellow liquor of soda and calcium alkali to be difficult to be utilized effectively.
At present, the main direction of development of chemical fertilizer is to develop composite fertilizer and slow-release fertilizer, phosphorus ammonia compound fertilizer (primary chemical into
It is divided into NH4H2PO4/(NH4)2HPO4) be widely used as a kind of outstanding quick-acting composite fertilizers, fertilising can provide plant life simultaneously
Nitrogen and phosphorus element needed for length.Ammonium magnesium phosphate (NH4MgPO4) it is a kind of efficient slow release fertilizer, because its is not soluble in water, not easily run off,
It is progressively absorbed for plant in the soil.Meanwhile ammonium magnesium phosphate also has extensive utilization in chemical industry, medicine, building field in itself.
The content of the invention
The purpose of the present invention is provided mainly for the problems of yellow liquor processing caused by solid base pulping process
Solid base is recycled while reducing discharge, can not only avoid complicated separation process, but also can realize that yellow liquor full constituent utilizes, is realized
The method of the recycling slurrying yellow liquor solid base coproduction organic ammonium quick-acting fertilizer and slow-release fertilizer of " zero-emission " target.
The present invention comprises the following steps：
1) fibre plant is after solid base pulping process boiling, and reaction product obtains paper pulp through separation of solid and liquid and slurrying is yellow
Liquid；
2) the slurrying yellow liquor in step 1) is heated to reflux, decomposes bicarbonate, solid content I and liquid are obtained through separation of solid and liquid
Body I；
3) ammonium hydroxide is added in into the liquid I that step 2) obtains, precipitation is generated, solid content II and filtrate is obtained after separation of solid and liquid
II；
4) ammonium hydroxide is added in the liquid I generated into step 2) to precipitation is no longer generated, solid content is obtained after separation of solid and liquid
III and filtrate II I；
5) by the solid content I that step 2) the obtains and solid content II that step 3) obtains or solid content III that step 4) obtains
Through cleaning, drying, roasting, solid base is recycled；
6) to step 3) obtain adding in the filtrate II I that filtrate II or step 4) obtain phosphoric acid to pH be 5~8, solid-liquid point
Solid content IV and filtrate IV are obtained from after；
7) dried after the solid content IV washings obtained step 6) to get slow-release fertilizer ammonium magnesium phosphate (NH4MgPO4)；
8) the filtrate IV that step 6) obtains is directly used as (the NH of ammonium salt containing lignin4 +- Lignin) and ammonium phosphate salt
(NH4H2PO4/(NH4)2HPO4) compound liquid fertilizer or it is concentrated, be granulated, it is dry after obtain lignin ammonium salt (NH4 +-
) and ammonium phosphate salt (NH Lignin4H2PO4/(NH4)2HPO4) compound fertilizer, (the NH of ammonium salt containing lignin4 +- Lignin) and phosphorus
Acid ammonium salt (NH4H2PO4/(NH4)2HPO4) compound liquid fertilizer and lignin ammonium salt (NH4 +- Lignin) and ammonium phosphate salt
(NH4H2PO4/(NH4)2HPO4) compound fertilizer be organic ammonium quick-acting fertilizer.
In step 2), the temperature being heated to reflux can be 100~150 DEG C.
In step 3), the mass percentage concentration of the ammonium hydroxide can be 25%~28%, and the addition of ammonium hydroxide is with liquid I's
Volume ratio can be 1 ︰ (6~20).
In step 4), the addition of the ammonium hydroxide is more than 1 ︰ 6 with the volume ratio of liquid I.
It is complicated that the present invention effectively overcomes in traditional boiling method yellow liquor treatment process, and the shortcomings that be difficult to efficiently use,
It can achieve the effect that full constituent utilizes, realize the environmental-friendly industrial theory of " zero-emission ".
Description of the drawings
Fig. 1 is ammonium magnesium phosphate TGA and the DSC collection of illustrative plates obtained by the embodiment of the present invention.In Fig. 1, curve a is Mass, curve b
For DSC.
Fig. 2 is the ammonium magnesium phosphate XRD spectrum obtained by the embodiment of the present invention.
Specific embodiment
The invention will be further described for example below, it is necessary to which explanation, embodiment is not formed will to the present invention
Ask the restriction of protection domain.
Embodiment 1
1kg (dry weight) fibre plant raw material is weighed, yellow liquor is collected after solid alkaline process pulping by cooking.Boiling yellow liquor is 150
It DEG C is heated to reflux, obtains reflux sediment and the yellow liquor that flows back, reflux yellow liquor dry weight account for liquid gross weight 7%.Into reflux yellow liquor
Industrial ammonia is added in by 1 ︰ 5 (volume ratio) additive amount, obtains ammonia process sediment.By reflux sediment and ammonia process sediment through removing
Miscellaneous, dry, roasting, is recycled solid base.It is 7.2 that industrial phosphoric acid is added in into ammonia process treated liquid to pH, obtains phosphorus
Sour magnesium ammonium precipitates, and raw phosphoric acid magnesium ammonium and phosphorus ammonia compound fertilizer solution are can obtain after separation of solid and liquid.Solid base yield is accounted in yellow liquor
The 68.5% of solid base total amount, ammonium magnesium phosphate yield are about the 7.8% of biomass addition, and phosphorus ammonia compound fertilizer dry weight accounts for biomass
The 31.7% of addition.
Embodiment 2
1kg (dry weight) fibre plant raw material is weighed, yellow liquor is collected after solid alkaline process pulping by cooking.Boiling yellow liquor is 110
It DEG C is heated to reflux, obtains reflux sediment and the yellow liquor that flows back.Into reflux yellow liquor industry is added in by 1 ︰ 10 (volume ratio) additive amount
Ammonium hydroxide obtains ammonia process sediment.Will reflux sediment and ammonia process sediment through cleaning, drying, roasting, be recycled solid base.
It is 5.5 that industrial phosphoric acid is added in into ammonia process treated liquid to pH, obtains ammonium magnesium phosphate precipitation, i.e. available after separation of solid and liquid
Raw phosphoric acid magnesium ammonium and phosphorus ammonia compound fertilizer solution.Solid base yield accounts for 61.5% of solid base total amount in yellow liquor, ammonium magnesium phosphate production
Amount is about the 5.5% of biomass addition, and phosphorus ammonia compound fertilizer dry weight accounts for the 25.1% of biomass addition.
Embodiment 3
1kg (dry weight) fibre plant raw material is weighed, yellow liquor is collected after solid alkaline process pulping by cooking.Boiling yellow liquor is 120
It DEG C is heated to reflux, obtains reflux sediment and the yellow liquor that flows back.Into reflux yellow liquor industry is added in by 1 ︰ 20 (volume ratio) additive amount
Ammonium hydroxide obtains ammonia process sediment.Will reflux sediment and ammonia process sediment through cleaning, drying, roasting, be recycled solid base.
It is 5.2 that industrial phosphoric acid is added in into ammonia process treated liquid to pH, obtains ammonium magnesium phosphate precipitation, i.e. available after separation of solid and liquid
Raw phosphoric acid magnesium ammonium and phosphorus ammonia compound fertilizer solution.Solid base yield accounts for 45.4% of solid base total amount in yellow liquor, ammonium magnesium phosphate production
Amount is about the 5.5% of biomass addition, and phosphorus ammonia compound fertilizer dry weight accounts for the 18.2% of biomass addition.
Ammonium magnesium phosphate TGA and DSC collection of illustrative plates obtained by the embodiment of the present invention referring to Fig. 1, join by the ammonium magnesium phosphate XRD spectrum of gained
See Fig. 2.
Claims (2)
1. recycle the method for slurrying yellow liquor solid base coproduction organic ammonium quick-acting fertilizer and slow-release fertilizer, it is characterised in that including following step
Suddenly：
1) for fibre plant after solid base pulping process boiling, reaction product obtains paper pulp and slurrying yellow liquor through separation of solid and liquid；
2) the slurrying yellow liquor in step 1) is heated to reflux, decomposes bicarbonate, solid content I and liquid I are obtained through separation of solid and liquid；
3) ammonium hydroxide is added in into the liquid I that step 2) obtains, precipitation is generated, solid content II and filtrate II is obtained after separation of solid and liquid；
The mass percentage concentration of the ammonium hydroxide is 25%~28%, the addition of ammonium hydroxide and the volume ratio of liquid I for 1 ︰ (6~
20)；
4) ammonium hydroxide is added in the liquid I generated into step 2) to precipitation is no longer generated, obtained after separation of solid and liquid solid content III and
Filtrate II I；
The addition of the ammonium hydroxide is more than 1 ︰ 6 with the volume ratio of liquid I；
5) by the solid content I that step 2) the obtains and solid content II that step 3) obtains or solid content III that step 4) obtains through removing
Miscellaneous, dry, roasting, recycles solid base；
6) to step 3) obtain adding in the filtrate II I that filtrate II or step 4) obtain industrial phosphoric acid to pH be 5~8, solid-liquid point
Solid content IV and filtrate IV are obtained from after；
7) dried after the solid content IV washings obtained step 6) to get slow-release fertilizer ammonium magnesium phosphate；
8) the filtrate IV that step 6) obtains is directly used as the compound liquid fertilizer of ammonium salt containing lignin and ammonium phosphate salt or through dense
Contracting, be granulated, it is dry after obtain the compound fertilizer of lignin ammonium salt and ammonium phosphate salt, the ammonium salt containing lignin and ammonium phosphate salt it is compound
Liquid fertilizer and the compound fertilizer of lignin ammonium salt and ammonium phosphate salt are organic ammonium quick-acting fertilizer.
2. the method for recycling slurrying yellow liquor solid base coproduction organic ammonium quick-acting fertilizer and slow-release fertilizer as described in claim 1, special
Sign is that in step 2) temperature being heated to reflux is 100~150 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611190506.9A CN106592312B (en) | 2016-12-21 | 2016-12-21 | The method for recycling slurrying yellow liquor solid base coproduction organic ammonium quick-acting fertilizer and slow-release fertilizer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611190506.9A CN106592312B (en) | 2016-12-21 | 2016-12-21 | The method for recycling slurrying yellow liquor solid base coproduction organic ammonium quick-acting fertilizer and slow-release fertilizer |
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| CN106592312A CN106592312A (en) | 2017-04-26 |
| CN106592312B true CN106592312B (en) | 2018-05-18 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1199796A (en) * | 1998-03-09 | 1998-11-25 | 乔凌星 | Comprehensive treating and utilizing method for papermaking black liquor |
| CN1436895A (en) * | 2002-02-09 | 2003-08-20 | 吴晓丽 | Comprehensive utilization method of pulping potash black liquor in paper-making process |
| CN101787656A (en) * | 2010-02-03 | 2010-07-28 | 中国科学院过程工程研究所 | Clean high-valued utilization method for straw resources |
| CN105332309A (en) * | 2015-10-09 | 2016-02-17 | 厦门大学 | Method for synchronically separating lignin and recovering solid alkali from solid alkali pulping waste liquid |
-
2016
- 2016-12-21 CN CN201611190506.9A patent/CN106592312B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1199796A (en) * | 1998-03-09 | 1998-11-25 | 乔凌星 | Comprehensive treating and utilizing method for papermaking black liquor |
| CN1436895A (en) * | 2002-02-09 | 2003-08-20 | 吴晓丽 | Comprehensive utilization method of pulping potash black liquor in paper-making process |
| CN101787656A (en) * | 2010-02-03 | 2010-07-28 | 中国科学院过程工程研究所 | Clean high-valued utilization method for straw resources |
| CN105332309A (en) * | 2015-10-09 | 2016-02-17 | 厦门大学 | Method for synchronically separating lignin and recovering solid alkali from solid alkali pulping waste liquid |
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| CN106592312A (en) | 2017-04-26 |
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