WO2014118600A1 - Method for production of compound fertilizers - Google Patents

Method for production of compound fertilizers Download PDF

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Publication number
WO2014118600A1
WO2014118600A1 PCT/IB2013/052345 IB2013052345W WO2014118600A1 WO 2014118600 A1 WO2014118600 A1 WO 2014118600A1 IB 2013052345 W IB2013052345 W IB 2013052345W WO 2014118600 A1 WO2014118600 A1 WO 2014118600A1
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WO
WIPO (PCT)
Prior art keywords
urea
sulphuric acid
slurry
mixing
production
Prior art date
Application number
PCT/IB2013/052345
Other languages
French (fr)
Inventor
Alfredas Martynas SVIKLAS
Vidmantas KUCINSKAS
Virginijus Streimikis
Original Assignee
UAB "ARVI" ir ko
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by UAB "ARVI" ir ko filed Critical UAB "ARVI" ir ko
Priority to EP13722082.8A priority Critical patent/EP2951136A1/en
Priority to EA201500269A priority patent/EA201500269A1/en
Publication of WO2014118600A1 publication Critical patent/WO2014118600A1/en

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES 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
    • C05G5/00Fertilisers characterised by their form
    • C05G5/10Solid or semi-solid fertilisers, e.g. powders
    • C05G5/12Granules or flakes

Definitions

  • the invention relates to the industry of mineral fertilizers and can be used in production of dry compound fertilizers (NPK), which involves use of urea.
  • NPK dry compound fertilizers
  • the invention further relates to use of hardening slurry for production of fertilizers and preparation of fertilizers having high total nitrogen concentration.
  • Urea is a concentrated nitrogen fertilizer with 46% of nitrogen, which can be used directly as a single nitrogen fertilizer or as a raw material for production of nitrogen, phosphorus and potassium (NPK) compound fertilizers.
  • a disadvantage of urea is that in water solutions (acid ones in particular) at relatively low temperatures (exceeding 50-60 o C) it undergoes hydrolysis and disintegrates into primary components: ammonia and carbon dioxide. This leads to nitrogen loss, environmental pollution, and necessity of additional equipment for cleaning of emissions.
  • the closest prior art is the European patent EP1127035 with priority date of 29 June 1998 and published on 6 January 2000 that describes a method for production of granulated compound fertilizer that consists of at least two basic nutrients: nitrogen, phosphorus and potassium.
  • the patent describes a method for the preparation of compound fertilizer granules by mixing solid raw materials with fine recycle material, melting a part of solid raw materials in a melter, mixing with remaining part of solid raw materials, granulating, cooling, screening, and packing. Throughout the process the dry components are moistened neither with water, nor with steam, therefore fertilizers are not dried. The drying stage is eliminated and thus the technological process gets simplified.
  • a disadvantage of this method is that energy consumption for melting some of the components (10-40%) is high: very hot air (200-550 o C) is supplied to the melter, moreover, components required for melting are additionally heated to reach the temperature of 80-110 o C.
  • total nitrogen concentration in compound fertilizers is not high, for example, fertilizer grade is 18-12-6, 17-17-17, there are no fertilizers needed for springtime fertilization.
  • the present invention is aimed to provide such a method for production of compound fertilizers that enables preparation of compound fertilizers with high nitrogen concentration in a simplified way, i.e., without a drying stage and with reduced energy consumption and atmospheric pollution.
  • the method for production of dry compound fertilizers that is being patented comprises mixing of dry components in a mixer and granulating of them.
  • up to 50 % of hardening slurry that supports the process of granulating can be fed into a mixer.
  • the optimal quantity is chosen by considering the nature and physical-chemical properties of raw materials and the ratio of components.
  • hardening slurry consisting of urea, sulphuric acid, magnesium and ammonium sulphate is additionally fed into the granulator wherein mass ratio of dry component and slurry is 1:0.1-0.6, preferably 1:0.2-0.5.
  • Preparation of hardening slurry comprises following three stages:
  • the magnesium component is melting product of periclase with MgO content of more than 75% and particle size of no more than 2 mm.
  • the method for preparation of compound fertilizers being patented simplifies the process and reduces energy consumption and atmospheric pollution as fertilizer drying is no longer necessary.
  • Fig. 1 shows a flow sheet of production of dry compound fertilizers.
  • Dry compound fertilizers are produced as shown in the flow sheet (Fig. 1). Dry components for fertilizer production are fed from bunkers (1) onto weighing scales (2), weighed and fed by mechanical feeders (3,5) and elevator (4) to mixer (6) and then to granulator (11). Hardening slurry produced in reactor I (7) by mixing urea with diluted sulphuric acid is also fed into granulator. The obtained urea and sulphuric acid slurry is (in) mixed with magnesium component in reactor II (8), slurry production is finished in reactor III (9) by adding ammonium sulphate. The obtained urea, sulphuric acid, magnesium and ammonium sulphate slurry is fed by pump (10) into granulator (11).
  • Granulated compound fertilizers are elevated by elevator (12) to sieve I (13) from which fine material is returned to mixer (6) and the remaining material is cooled in cooler (14), screened in sieve II (15), marketable part of the product is delivered to storage while the coarse material is crushed in crusher (16) and screened in sieve II (15).
  • Standard fertilizer analysis methods are used to determine concentrations of nitrogen, phosphorus, potassium, magnesium, sulphur and other elements in as well as physical-chemical properties and marketability indicators of dry compound fertilizers.
  • Compound fertilizers were produced in industrial-grade machine at output capacity of 10 tons per hour. Composition of dry substances and slurry used in production of dry compound fertilizers is illustrated by the following examples.

Abstract

The aim of this invention is to present such a method for production of compound fertilizers that simplifies the process and reduces energy consumption as well as atmospheric pollution. Water and/or water vapour are not used for moistening of the fertilizer components: this enables elimination of drying stage. This method for production of dry compound fertilizers features mixing of dry components in a mixer and subsequent granulating of them, additional feeding-in of hardening slurry consisting of urea, sulphuric acid, magnesium and ammonium sulphate into granulator. Preparation of hardening slurry comprises three stages: (a) mixing of urea with concentrated sulphuric acid and diluting with water; (b) mixing of the slurry obtained with magnesium component such as melting product of periclase; (c) mixing of the slurry obtained with ammonium sulphate. The use of present method for production of compound fertilizers leads to production of fertilizers having high concentration of nitrogen.

Description

METHOD FOR PRODUCTION OF COMPOUND FERTILIZERS Technical Field
The invention relates to the industry of mineral fertilizers and can be used in production of dry compound fertilizers (NPK), which involves use of urea. The invention further relates to use of hardening slurry for production of fertilizers and preparation of fertilizers having high total nitrogen concentration.
Background Art
Urea is a concentrated nitrogen fertilizer with 46% of nitrogen, which can be used directly as a single nitrogen fertilizer or as a raw material for production of nitrogen, phosphorus and potassium (NPK) compound fertilizers.
A disadvantage of urea is that in water solutions (acid ones in particular) at relatively low temperatures (exceeding 50-60oC) it undergoes hydrolysis and disintegrates into primary components: ammonia and carbon dioxide. This leads to nitrogen loss, environmental pollution, and necessity of additional equipment for cleaning of emissions.
There is a traditional method for production of granulated compound fertilizers, described in Fertilizer Manual, UNIDO (United Nations Industrial Development Organization, Vienna, IFDC, Alabama, 1980, 353 p.) wherein dry components (such as ammonium phosphates, ammonium nitrite, urea, ammonium sulphate, potassium chloride, superphosphate etc.) of conventional fertilizers are mixed, moistened with water and/or water vapour, granulated, dried, cooled, and fractioned. A disadvantage of this process is that urea reacts with potassium chloride and superphosphate and in the course of this gaseous and dust emissions that need to be cleaned forms. Moisture evaporation from fertilizers to achieve standard requirements requires energy, moreover, fertilizers with high concentration of nitrogen are not obtained.
There is a Russian patent RU2217399 with priority date of 22 August 2002 and published on 10 March 2004 that describes a method for production of compound fertilizers, which comprises thermal treating of urea with potassium sulphate and granulating it to produce nitrogen-potassium fertilizers. The method described in the patent offers simplified technological process, reduced number of stages, and lower losses of nitrogen. A disadvantage of this method is that fertilizers produced according to this method contain no phosphorus and the variety of fertilizers is very limited.
The closest prior art is the European patent EP1127035 with priority date of 29 June 1998 and published on 6 January 2000 that describes a method for production of granulated compound fertilizer that consists of at least two basic nutrients: nitrogen, phosphorus and potassium. The patent describes a method for the preparation of compound fertilizer granules by mixing solid raw materials with fine recycle material, melting a part of solid raw materials in a melter, mixing with remaining part of solid raw materials, granulating, cooling, screening, and packing. Throughout the process the dry components are moistened neither with water, nor with steam, therefore fertilizers are not dried. The drying stage is eliminated and thus the technological process gets simplified. A disadvantage of this method is that energy consumption for melting some of the components (10-40%) is high: very hot air (200-550oC) is supplied to the melter, moreover, components required for melting are additionally heated to reach the temperature of 80-110oC. In addition, regardless of the use of urea, total nitrogen concentration in compound fertilizers is not high, for example, fertilizer grade is 18-12-6, 17-17-17, there are no fertilizers needed for springtime fertilization.
Accordingly there is a need for production of such compound fertilizers that can be prepared in a simplified way while decreasing energy consumption and atmospheric pollution and increasing nitrogen concentration in fertilizers.
Technical Solution
The present invention is aimed to provide such a method for production of compound fertilizers that enables preparation of compound fertilizers with high nitrogen concentration in a simplified way, i.e., without a drying stage and with reduced energy consumption and atmospheric pollution.
The method for production of dry compound fertilizers that is being patented comprises mixing of dry components in a mixer and granulating of them.
Alternatively, in accordance with present invention up to 50 % of hardening slurry that supports the process of granulating can be fed into a mixer. The optimal quantity is chosen by considering the nature and physical-chemical properties of raw materials and the ratio of components.
To simplify the process and to reduce energy consumption and atmospheric pollution, hardening slurry, consisting of urea, sulphuric acid, magnesium and ammonium sulphate is additionally fed into the granulator wherein mass ratio of dry component and slurry is 1:0.1-0.6, preferably 1:0.2-0.5.
Next, the granules are cooled down, screened, fine material is returned to mixer wherein mass ratio of dry component and fine material is 1:0.5-4.
Later granules are conditioned and delivered to storage. The produced product is carried for 24-36 hours in the storage until fertilizer hygroscopic water content of 1-1.5% is achieved.
Preparation of hardening slurry comprises following three stages:
  1. (a) mixing of urea for up to 5 minutes with concentrated sulphuric acid at mass ratio of 1:0.05-0.2, preferably at mass ratio of 1:0.1-0.2, diluting with water at mass ratio of sulphuric acid to water of 1: 0.5-1.0 at the temperature of 45-50o C until density of 1.35-1.39 g/cm3 and pH of less than 1.5 are achieved;
  1. (b) mixing the slurry obtained with magnesium component at mass ratio of urea:MgO:sulphuric acid of 1:0.05-0.2:0.05-0.2, preferably at mass ratio of 1:0.09-0.11:0.09-0.11, maintaining slurry pH of 3.5-5.5 at the temperature of 75-85o C;
  1. (c) mixing slurry of the urea, sulphuric acid, and magnesium components obtained with ammonium sulphate at the temperature of 75-90o C and the pH of 4.5-6.5.
In accordance with the embodiment of present invention the magnesium component is melting product of periclase with MgO content of more than 75% and particle size of no more than 2 mm.
The method for preparation of compound fertilizers being patented simplifies the process and reduces energy consumption and atmospheric pollution as fertilizer drying is no longer necessary.
Description of Drawings
Fig. 1 shows a flow sheet of production of dry compound fertilizers.
Best Mode
Dry compound fertilizers are produced as shown in the flow sheet (Fig. 1). Dry components for fertilizer production are fed from bunkers (1) onto weighing scales (2), weighed and fed by mechanical feeders (3,5) and elevator (4) to mixer (6) and then to granulator (11). Hardening slurry produced in reactor I (7) by mixing urea with diluted sulphuric acid is also fed into granulator. The obtained urea and sulphuric acid slurry is (in) mixed with magnesium component in reactor II (8), slurry production is finished in reactor III (9) by adding ammonium sulphate. The obtained urea, sulphuric acid, magnesium and ammonium sulphate slurry is fed by pump (10) into granulator (11). Part of the slurry can be fed into the mixer (6) as well. Granulated compound fertilizers are elevated by elevator (12) to sieve I (13) from which fine material is returned to mixer (6) and the remaining material is cooled in cooler (14), screened in sieve II (15), marketable part of the product is delivered to storage while the coarse material is crushed in crusher (16) and screened in sieve II (15).
If it is desirable to add microelements or other plant nutrients to fertilizers produced, then these are loaded to bunkers (1).
Standard fertilizer analysis methods are used to determine concentrations of nitrogen, phosphorus, potassium, magnesium, sulphur and other elements in as well as physical-chemical properties and marketability indicators of dry compound fertilizers.
Compound fertilizers were produced in industrial-grade machine at output capacity of 10 tons per hour. Composition of dry substances and slurry used in production of dry compound fertilizers is illustrated by the following examples.
Example 1. 18-18-18-2MgO-2S
Raw material Composition, % Quantity, kg/t
Slurry
Ammonium sulphate 20.5 N 25.0
Urea 46.0 N 160.0
Magnesite 85.0 MgO 17.0
Sulphuric acid 98.0 26.0
Water 17.0
245.0
Dry raw materials
Ammonium sulphate 20.5 N 8.2
Urea 46.0 N 60.8
Diammophos (DAP) 18.0 N, 46.0 P2O5 387.0
KCl (MOP) 60.0 K2O 297.0
Wax 2.0
755.0
Total: 1000.0
Example 2. 25-6-6-2MgO-8S
Raw material Composition, % Quantity, kg/t
Slurry
Ammonium sulphate 20.5 N 40.0
Urea 46.0 N 200.0
Magnesite 85.0 MgO 22.0
Sulphuric acid 98.0 34.0
Water 21.0
317.0
Dry raw materials
Ammonium sulphate 20.5 N 317.4
Urea 46.0 N 133.2
Diammophos (DAP) 18.0 N, 46.0 P2O5 130.4
KCl (MOP) 60.0 K2O 100.0
Wax 2.0
683.0
Total: 1000.0
Example 3. 27-5-6-2.5MgO-6S
Raw material Composition, % Quantity, kg/t
Slurry
Ammonium sulphate 20.5 N 46.7
Urea 46.0 N 300.0
Magnesite 85.0 MgO 32.7
Sulphuric acid 98.0 48.2
Water 31.1
458.7
Dry raw materials
Ammonium sulphate 20.5 N 193.0
Urea 46.0 N 137.7
Diammophos (DAP) 18.0 N, 46.0 P2O5 108.6
KCl (MOP) 60.0 K2O 100.0
Wax 2.0
541.3
Total: 1000.0
Example 4. 32-5-5-2.5MgO-2S
Raw material Composition, % Quantity, kg/t
Slurry
Ammonium sulphate 20.5 N 46.7
Urea 46.0 N 300.0
Magnesite 85.0 MgO 32.7
Sulphuric acid 98.0 48.2
Water 31.1
458.7
Dry raw materials
Ammonium sulphate 20.5 N 26.9
Urea 46.0 N 320.4
Diammophos (DAP) 18.0 N, 46.0 P2O5 108.7
KCl (MOP) 60.0 K2O 83.3
Wax 2.0
541.3
Total: 1000.0
The following technological parameters were maintained during production:
  1. - granulation temperature 35-50o C,
  1. - temperature of cooled fertilizer 18-40o C,
  1. - strength of granules of compound fertilizer 3.2-4.5 MPa,
  1. - hygroscopic water content in product 3.2-4.0 % (right after production),
1.0-1.5 % (after 36 h),
  1. - fractional composition of product (2-5 mm) at least 98 %.
To illustrate and describe this invention, descriptions of preferred embodiments are given above. This is not a complete or limiting invention aimed at prescribing a precise embodiment or implementation option. The description given above should be regarded more as an illustration than a constraint. Obviously, the person skilled in the art may clearly see a multitude of modifications and variations. The preferred embodiments have been selected and described so as to enable the person skilled in the art to best understand the principles behind this invention and their best practical application for different embodiments with different modifications fit for a specific application or implementation customisation, because in each particular case there may be different quantitative indicators relating to application of this method. The invention scope is defined by the attached definition and its equivalents wherein all the terms used have the broadest possible meanings unless stated otherwise. It must be admitted that implementation options described by the person skilled in the art may contain changes that do not depart from the scope of this invention, as described in the definition given next.

Claims (10)

1. Method for production of dry compound fertilizers by mixing of dry components of nitrogen, phosphorus, and potassium in a mixer, granulating and screening of them, returning fine material to mixer and conditioning it, characterized in that to simplify the process and to reduce energy consumption hardening slurry consisting of urea, sulphuric acid, magnesium and ammonium sulphate is fed into the granulator.
2. Method according to claim 1, characterized in that up to 50% of hardening slurry can also be fed into a mixer.
3. Method according to claims 1 and 2, characterized in that mass ratio of fertilizer dry component and hardening slurry is 1:0.1-0.6, preferable 1:0.2-0.5.
4. Method according to any of the claims 1‑3, characterized in that mass ratio of fertilizer dry component in mixer and fine recycle material is 1:0.5-4.
5. Method according to any of the claims 1‑4, characterized in that preparation of hardening slurry comprises three stages:
(a) mixing of urea with concentrated sulphuric acid and diluting with water;
(b) mixing of the slurry of urea and sulphuric acid obtained with magnesium component;
(c) mixing of the slurry of urea, sulphuric acid, and magnesium components obtained with ammonium sulphate.
6. Method according to any of the claims 1‑5, characterized in that at stage (a) urea is mixed for up to 5 minutes with concentrated sulphuric acid at mass ratio of urea:sulphuric acid of 1:0.05‑0.2, preferably of 1:0.1‑0.2; and diluted with water at mass ratio of sulphuric acid:water of 1:0.5‑1.0 at the temperature of 45‑50o C until suspension density of 1.35‑1.39 g/cm3 and pH of less than 1.5 are achieved.
7. Method according to any of the claims 1‑6, characterized in that magnesium component is mixed with stage (a) slurry of urea and sulphuric acid at mass ratio of urea:MgO:sulphuric acid of 1:0.05-0.2:0.05-0.2, preferably at mass ratio of 1:0.09-0.11:0.09-0.11, maintaining slurry pH of 3.5-5.5 at the temperature of 75‑85o C.
8. Method according to claim 7, characterized in that at stage (b) slurry is mixed with magnesium component such as melting product of periclase with MgO content of at least 75% and particle size of no more than 2 mm.
9. Method according to any of the preceding claims, characterized in that at stage (c) slurry of urea, sulphuric acid, and magnesium components is mixed with ammonium sulphate at the temperature of 75-90o C and the pH of 4.5-6.5.
10. Method according to any of the preceding claims, characterized in that the produced product is carried in the storage for 24-36 hours.
PCT/IB2013/052345 2013-01-31 2013-03-25 Method for production of compound fertilizers WO2014118600A1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP13722082.8A EP2951136A1 (en) 2013-01-31 2013-03-25 Method for production of compound fertilizers
EA201500269A EA201500269A1 (en) 2013-01-31 2013-03-25 METHOD OF MANUFACTURING MIXED FERTILIZERS

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
LT2013007A LT5974B (en) 2013-01-31 2013-01-31 Process for preparing compound fertilizer
LT2013-007 2013-01-31

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EA (1) EA201500269A1 (en)
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WO (1) WO2014118600A1 (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106040152A (en) * 2016-07-01 2016-10-26 明辉大秦(上海)环保科技有限公司 Automatic production equipment of high-performance fast-dissolved adhesive powder
CN106040151A (en) * 2016-07-01 2016-10-26 明辉大秦(上海)环保科技有限公司 Semi-automatic production device of high-performance fast-dissolved adhesive powder
RU216422U1 (en) * 2022-11-23 2023-02-02 федеральное государственное бюджетное образовательное учреждение высшего образования "Южно-Российский государственный политехнический университет (НПИ) имени М.И. Платова" granulation tower

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115183537A (en) * 2022-07-18 2022-10-14 赤壁市高质量发展研究院有限公司 Method for reducing water vapor saturation in drying cylinder

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Publication number Priority date Publication date Assignee Title
US5264017A (en) * 1988-01-06 1993-11-23 Martin Marietta Magnesia Specialties Inc. Inorganic reactive granulating binder and conditioner
US6254655B1 (en) * 1999-03-18 2001-07-03 Oms Investments, Inc. Processes for preparing granular composite fertilizer compositions and products produced thereby
EP1127035A1 (en) 1998-06-29 2001-08-29 Kemira Agro Oy A process for the preparation of compound fertilizer granules
RU2217399C1 (en) 2002-08-22 2003-11-27 Пойлов Владимир Зотович Method for preparing nitrogen-potassium-sulfate fertilizer
EP2017242A1 (en) * 2006-05-11 2009-01-21 Iniciativas Agroindustriales de Teruel, S.L. Methods for obtaining nitrogenated fertilizers and complexes and fertilizers thus obtained

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5264017A (en) * 1988-01-06 1993-11-23 Martin Marietta Magnesia Specialties Inc. Inorganic reactive granulating binder and conditioner
EP1127035A1 (en) 1998-06-29 2001-08-29 Kemira Agro Oy A process for the preparation of compound fertilizer granules
US6254655B1 (en) * 1999-03-18 2001-07-03 Oms Investments, Inc. Processes for preparing granular composite fertilizer compositions and products produced thereby
RU2217399C1 (en) 2002-08-22 2003-11-27 Пойлов Владимир Зотович Method for preparing nitrogen-potassium-sulfate fertilizer
EP2017242A1 (en) * 2006-05-11 2009-01-21 Iniciativas Agroindustriales de Teruel, S.L. Methods for obtaining nitrogenated fertilizers and complexes and fertilizers thus obtained

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106040152A (en) * 2016-07-01 2016-10-26 明辉大秦(上海)环保科技有限公司 Automatic production equipment of high-performance fast-dissolved adhesive powder
CN106040151A (en) * 2016-07-01 2016-10-26 明辉大秦(上海)环保科技有限公司 Semi-automatic production device of high-performance fast-dissolved adhesive powder
CN106040152B (en) * 2016-07-01 2018-06-26 明辉大秦(上海)环保科技有限公司 A kind of automated production equipment of high-performance instant dissolving glue powder
CN106040151B (en) * 2016-07-01 2018-08-31 明辉大秦(上海)环保科技有限公司 A kind of semi-automatic process units of high-performance instant dissolving glue powder
RU216422U1 (en) * 2022-11-23 2023-02-02 федеральное государственное бюджетное образовательное учреждение высшего образования "Южно-Российский государственный политехнический университет (НПИ) имени М.И. Платова" granulation tower

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Publication number Publication date
LT5974B (en) 2013-11-25
LT2013007A (en) 2013-08-26
EP2951136A1 (en) 2015-12-09
EA201500269A1 (en) 2016-06-30

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