CN106592312A - Method for recovering solid alkali from pulping yellow liquid for coproduction of organic ammonium quick-acting fertilizer and slow release fertilizer - Google Patents
Method for recovering solid alkali from pulping yellow liquid for coproduction of organic ammonium quick-acting fertilizer and slow release fertilizer Download PDFInfo
- Publication number
- CN106592312A CN106592312A CN201611190506.9A CN201611190506A CN106592312A CN 106592312 A CN106592312 A CN 106592312A CN 201611190506 A CN201611190506 A CN 201611190506A CN 106592312 A CN106592312 A CN 106592312A
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- Prior art keywords
- solid
- liquid
- fertilizer
- ammonium
- solid content
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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
Abstract
The invention discloses a method for recovering solid alkali from a pulping yellow liquid for coproduction of organic ammonium quick-acting fertilizer and slow release fertilizer. After fiber plants are cooked with a solid alkali pumping method, paper pulp and the pulping yellow liquid are obtained through solid-liquid separation of a reaction product; the pulping yellow liquid is subjected to heating reflux for decomposition of bicarbonate, and a solid content I and a liquid I are obtained after solid-liquid separation; ammonia water is added to the liquid I, precipitate is produced, and a solid content II and a filtrate II are obtained after solid-liquid separation; ammonia water is added to the liquid I until no precipitate is produced, and a solid content III and a filtrate III are obtained after solid-liquid separation; the solid content I and the solid content II or the solid content III are subjected to impurity removal, drying and roasting for recovery of solid alkali; phosphoric acid is added to the filtrate II or the filtrate III until the pH ranges from 5 to 8, and a solid content IV and a filtrate IV are obtained after solid-liquid separation; the solid content IV is washed and then dried, and slow release fertilizer ammonium magnesium phosphate is obtained; the filtrate IV is used as compound liquid fertilizer or ammonium lignin and ammonium phosphate compound fertilizer is obtained after concentration, granulation and drying.
Description
Technical field
The present invention relates to chemical fertilizer, more particularly, to it is a kind of reclaim 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, the method will accelerate cleaning pulping and prepare high level chemicals
Etc. the industrialization of biomass energy Chemical Engineering Technology.Chinese patent CN105332309A discloses a kind of same from solid base slurrying yellow liquor
One-step separation of wood quality and the method for reclaiming solid base, the method is that the process of solid base slurrying yellow liquor and the recovery of effective ingredient are carried
Good thinking has been supplied, but it adopts soda and the remaining yellow liquor of calcium alkali to be difficult to be utilized effectively.
At present, the main development direction of chemical fertilizer is development compound 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 compound fertilizer, fertilising can simultaneously provide plant life
Nitrogen, P elements needed for long.Ammonium magnesium phosphate (NH4MgPO4) it is a kind of efficient slow release fertilizer, it is water insoluble because of its, not easily run off,
Progressively absorb for plant in soil.Meanwhile, ammonium magnesium phosphate sheet also has extensive utilization in chemical industry, medicine, building field.
The content of the invention
The purpose of the present invention is mainly for the problems of yellow liquor process produced by solid base pulping process, there is provided
Solid base is reclaimed while reducing discharge, the separation process of complexity can have both been avoided, yellow liquor full constituent is capable of achieving again and is utilized, realized
The method for reclaiming slurrying yellow liquor solid base coproduction organic ammonium quick-acting fertilizer and slow-release fertilizer of " zero-emission " target.
The present invention is comprised the following steps：
1) fibre plant is Jing after solid base pulping process steaming and decocting, and product Jing solid-liquid separation obtains paper pulp and slurrying is yellow
Liquid；
2) by step 1) in slurrying yellow liquor be heated to reflux, decompose bicarbonate, Jing solid-liquid separation obtains solid content I and liquid
Body I；
3) to step 2) ammonia is added in the liquid I that obtains, precipitation is produced, solid content II and filtrate are obtained after solid-liquid separation
II；
4) to step 2) in produce liquid I in add ammonia to no longer produce precipitation, solid content is obtained after solid-liquid separation
III and filtrate II I；
5) by step 2) the solid content I that obtains and step 3) the solid content II that obtains or step 4) the solid content III that obtains
Jing remove impurity, drying, roasting, reclaim solid base；
6) to step 3) obtain filtrate II or step 4) add phosphoric acid to be 5～8 to pH in filtrate II I that obtains, solid-liquid point
Solid content IV and filtrate IV is obtained after；
7) by step 6) it is dried after the solid content IV that obtains washing, obtain final product slow-release fertilizer ammonium magnesium phosphate (NH4MgPO4)；
8) by step 6) the filtrate IV that obtains is directly used as (the NH of ammonium salt containing lignin4 +- Lignin) and ammonium phosphate salt
(NH4H2PO4/(NH4)2HPO4) compound liquid fertilizer, or lignin ammonium salt (NH is obtained after concentrated, pelletize, drying4 +-
) 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) in, the temperature being heated to reflux can be 100～150 DEG C.
In step 3) in, the mass percentage concentration of the ammonia can be 25%～28%, and the addition of ammonia is with liquid I's
Volume ratio can be 1 ︰ (6～20).
In step 4) in, the addition of the ammonia is more than 1 ︰ 6 with the volume ratio of liquid I.
The present invention effectively overcomes in traditional boiling method that yellow liquor treatment process is complicated, and is difficult to the shortcoming of effectively utilizes,
The effect that full constituent is utilized can be reached, the environmental friendliness industry theory of " zero-emission " is realized.
Description of the drawings
Fig. 1 is the ammonium magnesium phosphate TGA and DSC collection of illustrative plates obtained by the embodiment of the present invention.In FIG, 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 should be noted that embodiment is not constituted wanting to the present invention
Ask the restriction of protection domain.
Embodiment 1
1kg (dry weight) fibre plant raw material is weighed, Jing after solid alkaline process pulping by cooking yellow liquor is collected.Steaming and decocting yellow liquor is 150
DEG C it is heated to reflux, obtains flow back precipitate and backflow yellow liquor, backflow yellow liquor dry weight accounts for liquid gross weight 7%.To in backflow yellow liquor
Industrial ammonia is added by 1 ︰ 5 (volume ratio) addition, ammonia process precipitate is obtained.Backflow precipitate and ammonia process precipitate Jing are removed
Miscellaneous, dry, roasting, is recycled solid base.Add industrial phosphoric acid to be 7.2 to pH in the liquid after ammonia process process, obtain phosphorus
Sour magnesium ammonium precipitation, is obtained raw phosphoric acid magnesium ammonium and phosphorus ammonia compound fertilizer solution after solid-liquid separation.Solid base yield is accounted in yellow liquor
The 68.5% of solid base total amount, ammonium magnesium phosphate yield is 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, Jing after solid alkaline process pulping by cooking yellow liquor is collected.Steaming and decocting yellow liquor is 110
DEG C it is heated to reflux, obtains flow back precipitate and backflow yellow liquor.Industry is added in backflow yellow liquor by 1 ︰ 10 (volume ratio) addition
Ammonia, obtains ammonia process precipitate.To be flowed back precipitate and ammonia process precipitate Jing remove impurity, drying, roasting, be recycled solid base.
Add industrial phosphoric acid to be 5.5 to pH in the liquid after ammonia process process, obtain ammonium magnesium phosphate precipitation, be obtained after solid-liquid separation
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, and ammonium magnesium phosphate is produced
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, Jing after solid alkaline process pulping by cooking yellow liquor is collected.Steaming and decocting yellow liquor is 120
DEG C it is heated to reflux, obtains flow back precipitate and backflow yellow liquor.Industry is added in backflow yellow liquor by 1 ︰ 20 (volume ratio) addition
Ammonia, obtains ammonia process precipitate.To be flowed back precipitate and ammonia process precipitate Jing remove impurity, drying, roasting, be recycled solid base.
Add industrial phosphoric acid to be 5.2 to pH in the liquid after ammonia process process, obtain ammonium magnesium phosphate precipitation, be obtained after solid-liquid separation
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, and ammonium magnesium phosphate is produced
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 is joined referring to Fig. 1, the ammonium magnesium phosphate XRD spectrum of gained
See Fig. 2.
Claims (4)
1. the method for reclaiming 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) fibre plant Jing after solid base pulping process steaming and decocting, product Jing solid-liquid separation obtains paper pulp and slurrying yellow liquor；
2) by step 1) in slurrying yellow liquor be heated to reflux, decompose bicarbonate, Jing solid-liquid separation obtains solid content I and liquid I；
3) to step 2) ammonia is added in the liquid I that obtains, precipitation is produced, solid content II and filtrate II are obtained after solid-liquid separation；
4) to step 2) in produce liquid I in add ammonia to no longer produce precipitation, obtain after solid-liquid separation solid content III and
Filtrate II I；
5) by step 2) the solid content I that obtains and step 3) the solid content II that obtains or step 4) the solid content III Jing that obtain remove
Miscellaneous, dry, roasting, reclaims solid base；
6) to step 3) obtain filtrate II or step 4) add industrial phosphoric acid to be 5～8 to pH in filtrate II I that obtains, solid-liquid point
Solid content IV and filtrate IV is obtained after；
7) by step 6) it is dried after the solid content IV that obtains washing, obtain final product slow-release fertilizer ammonium magnesium phosphate；
8) by step 6) the filtrate IV that obtains is directly used as the compound liquid fertilizer of ammonium salt containing lignin and ammonium phosphate salt, or Jing dense
The compound of the compound fertilizer of lignin ammonium salt and ammonium phosphate salt, the ammonium salt containing lignin and ammonium phosphate salt is obtained after contracting, pelletize, drying
The compound fertilizer of liquid fertilizer and lignin ammonium salt and ammonium phosphate salt is organic ammonium quick-acting fertilizer.
2. the method for reclaiming slurrying yellow liquor solid base coproduction organic ammonium quick-acting fertilizer and slow-release fertilizer as claimed in claim 1, it is special
Levy is in step 2) in, the temperature being heated to reflux is 100～150 DEG C.
3. the method for reclaiming slurrying yellow liquor solid base coproduction organic ammonium quick-acting fertilizer and slow-release fertilizer as claimed in claim 1, it is special
Levy is in step 3) in, the mass percentage concentration of the ammonia is 25%～28%, the addition of ammonia and the volume of liquid I
Than for 1 ︰ (6～20).
4. the method for reclaiming slurrying yellow liquor solid base coproduction organic ammonium quick-acting fertilizer and slow-release fertilizer as claimed in claim 1, it is special
Levy is in step 4) in, the addition of the ammonia is more than 1 ︰ 6 with the volume ratio of liquid I.
Priority Applications (1)
| 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 |
Applications Claiming Priority (1)
| 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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106592312A true CN106592312A (en) | 2017-04-26 |
| CN106592312B CN106592312B (en) | 2018-05-18 |
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| CN201611190506.9A Active 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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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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| CN106592312B (en) | 2018-05-18 |
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