GB1584703A - Process for the preparation of sodium bisulphate granules - Google Patents
Process for the preparation of sodium bisulphate granules Download PDFInfo
- Publication number
- GB1584703A GB1584703A GB38193/79A GB3819379A GB1584703A GB 1584703 A GB1584703 A GB 1584703A GB 38193/79 A GB38193/79 A GB 38193/79A GB 3819379 A GB3819379 A GB 3819379A GB 1584703 A GB1584703 A GB 1584703A
- Authority
- GB
- United Kingdom
- Prior art keywords
- sodium bisulphate
- granules
- temperature
- granulation
- carried out
- Prior art date
- Legal status (The legal status 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 status listed.)
- Expired
Links
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 title claims description 25
- 238000000034 method Methods 0.000 title claims description 22
- 239000008187 granular material Substances 0.000 title claims description 19
- 238000002360 preparation method Methods 0.000 title claims description 6
- 238000005469 granulation Methods 0.000 claims description 13
- 230000003179 granulation Effects 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000001816 cooling Methods 0.000 description 10
- 239000000155 melt Substances 0.000 description 10
- 238000005507 spraying Methods 0.000 description 7
- 230000009466 transformation Effects 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 3
- 238000007654 immersion Methods 0.000 description 2
- 230000001131 transforming effect Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-M bisulphate group Chemical group S([O-])(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- -1 salt hydrates Chemical class 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/02—Preparation of sulfates from alkali metal salts and sulfuric acid or bisulfates; Preparation of bisulfates
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Glanulating (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Fertilizers (AREA)
Description
PATENT SPECIFICATION
( 21) ( 62) Application No 38193/79 Divided out of No 1 584 702 ( 31) Convention Application No.
2 619 811 ( 33) Fed Rep of Germany (DE) ( 22) Filed 4 May 1977 ( 32) Filed 5 May 1976 in ( 44) Complete Specification published 18 Feb 1981 ( 51) INT CL 3 C Ol D 5/02 ( 52) Index at acceptance C 1 A D 19 G 5 OG 50 D 19 PF 5 ( 54) PROCESS FOR THE PREPARATION OF SODIUM BISULPHATE GRANULES ( 71) We, HOECHST AKTIENGESELLSCHAFT, a body corporate organised according to the laws of the Federal Republic of Germany, of 6230 Frankfurt/Main 80, Postfach 80 03 20, Federal Republic of Germany, do hereby declare the invention for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement:-
The present invention relates to the preparation of sodium bisulphate granules.
Granulation of sodium bisulphate may for example be carried out by transforming into scales or by spraying in a cooling tower or on to a cooling strip It has been ascertained, however, that the granulated sodium bisulphate produced from a melt is mainly present in a vitreous, metastable state, and therefore it can be processed only with difficulty When this granulated product is stored in silos, barrels or sacks, its metastable phase is transformed into the stable phase over approximately 24 hours, and a considerable quantity of heat is evolved whereby the temperature may increase by up to 100 C At the same time the product hardens to such a degree that it can be transformed into a form ready for use only with considerable expenditure, by crushing and sieving it Freshly granulated product in the metastable state can also only be crushed with difficulty, as it behaves like a tough mass There is therefore a need to transform the granules largely or entirely into a stable form prior to storage or further processing.
The invention provides a process for the preparation of sodium bisulphate granules which comprises granulating molten sodium bisulphate and subsequently keeping the granulated product for at least one minute at a temperature in the range of from 60 to 1400 C The resulting product consists of non-sticking granules.
The melt may be granulated in any suitable manner, for example by spraying in a spray tower (whereby the liquid bisulphate solidifies during the free fall), by solidification on a cooling strip or on a scale roll.
The transformation into the stable phase in the given temperature range takes place faster the higher the temperature At a temperature of from 50 to 600 C the transformation requires about 24 hours, at a 55 temperature of 100 'C about 10 minutes and at a temperature of from 120 to 1400 C about 1 minute The transformation should not be carried out below 60 C, since long residence times are not very economical A 60 temperature in the range of from 120 to C is preferred.
A product which has not been stabilized may be subject to a sudden temperature increase accompanied by agglomeration, 65 even after several days, whereas the stabilized granulate is storable without difficulty over a long period of time.
By the process of the present invention the transformation of the metastable form 70 of granulated sodium bisulphate into the stable form is accelerated.
The transformation of the metastable sodium bisulphate into the stable form can also be accelerated by increasing the water 75 content of the melt to 0 01 to 3 % by weight of water, prior to granulation, and this can be carried out in addition to the abovedescribed post-granulation treatment of the invention Non-sticking granules are 80 produced.
This variant of the process according to the invention is applicable, for example, to granulation on a scale roll, and, preferably, to spraying in a cooling tower, whereby the 85 molten sodium bisulphate solidifies during the free fall It is thought that, in the presence of water, primary salt hydrates are formed which act as catalyst for the transformation of the metastable phase into the 90 stable phase.
This treatment may be carried out for example as follows:
4000 kg per hour of sodium bisulphate melt (content of sodium bisulphate 96 5 %) 95 are produced in a circulation reactor The melt is sprayed in the cooling tower (quantity of steam 20 kg per hour) by means of bi-component nozzles.
The product obtained is substantially 100 m N x_ GC ( 11) 1 584 703 D 19 1 584 703 stable and can be further processed without difficulty (water content: 0 15 %) according to the process of the invention.
For transforming the metastable form of sodium bisulphate into the stable form, it has moreover proved advantageous to adjust the temperature of the melt prior to granulating to be within a well defined range, from 186 to 2360 C whereby nonsticking granules are produced The cooling speed in 'C per unit of time is lower in this temperature range than when cooling a melt which has a temperature of from 240 to 280 WC to the same final temperature and, as a consequence thereof, most of the sodium bisulphate solidifies in the desired stable phase This applies especially to granulation in a spraying tower This process can be carried out in addition to the post-granulation treatment of the invention, and if desired as well as increasing the water content.
This pre-granulation treatment may be carried out for example as follows:
1100 1 of technical grade sulphuric acid (d = 1 84) and 1200 kg of marine salt are fed into a circulation reactor per hour to produce a sodium bisulphate melt The temperature of the melt is maintained at 260 C by burning 210 m 3/hour of hydrogen with air in an immersion heater On its way to the spraying tower the melt is cooled to 220 WC by a cooled tube mounted directly before the spra in nozzles The granules are cooled to 400 C by cooling air in the spraying tower.
These granules only have a moderate tendency to get sticky and can subsequently be further processed according to the process of the invention without essential difficulties.
The above methods for the transformation of metastable sodium bisulphate give maximum useful yields from a given reactor.
They are suitable for the granulation of products produced in a submerged combustion burner, a circulation reactor which circulates the melt, directly heated by means of an immersion heater, and also for products obtained from processes for the preparation of fluid sodium bisulphate The melt may be produced, for example, by the process described and claimed in our copending application no 18660/77 (Serial No 1 584 702).
The following Examples 1 and 2 illustrate the invention:
Comparative Example A sodium bisulphate melt at 260 WC was sprayed in a cooling tower through nozzles and the solidified granules were cooled to 350 C by means of cold air and then stored in containers Over several hours, the product was subject to a self-heating to about 1250 C, whereby the product agglomerated forming blocks as hard as stone Consequently, the product was not suitable for further use.
EXAMPLE 1:
The procedure was analogous to that in the comparative Example, except that the temperature of the solidified granules was adjusted to about 650 C by reducing the 70 quantity of cooling air during spraying and by preheating the air Moreover, the product was stored at this temperature for about 40 minutes The solidified granules remained free flowing even after several 75 weeks and could readily be further processed.
EXAMPLE 2:
The operation was analogous to that of the comparative Example, except that the 80 solidified granules were cooled only to a temperature of about 1000 C during granulation The temperature of 100 TC was maintained for 10 minutes This residence time was sufficient for the complete transforma 85 tion of the metastable sodium bisulphate.
Even after a rather long period of time the product did not agglomerate.
Claims (1)
- WHAT WE CLAIM IS:1 A process for the preparation of 90 sodium bisulphate granules from molten sodium bisulphate, which comprises granulating the molten sodium bisulphate and subsequently holding the granules for at least one minute at a temperature in the 95 range of from 60 to 140 C.2 A process as claimed in claim 1, wherein the granules are held at a temperature in the range of from 120 to 140 C.3 A process as claimed in claim 1 or 100 claim 2, wherein granulation is carried out in a spray tower.4 A process as claimed in claim 1, carried out substantially as described in either Example 1 or Example 2 herein 105 A process as claimed in any one of claims 1 to 4, wherein granulation of the molten sodium bisulphate is carried out in the presence of from 0 01 to 3 % by weight of water 110 6 A process as claimed in claim 5, wherein water is added substantially as described herein.7 A process as claimed in any one of claims 1 to 6, wherein the temperature of 115 the molten sodium bisulphate is adjusted to be in the range of from 186 to 236 C before granulation from this temperature.8 A process as claimed in claim 7, wherein the pre-granulation temperature 120 adjustment is carried out substantially as described herein.9 Sodium bisulphate granules, whenever prepared by a process as claimed in any one of claims 1 to 8 125 ABEL & IMRAY Chartered Patent Agents, Northumberland House, 303-306 High Holborn, London, WC 1 V 7 LH.3 1 584703 3 Printed for Her Majesty's Stationery Office by The Tweeddale Press Ltd, Berwick-upon-Tweed, 1980 Published at the Patent Office, 25 Southampton Buildings, London, WC 2 A l AY, from which copies may be obtained.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE2619811A DE2619811C2 (en) | 1976-05-05 | 1976-05-05 | Process for the production of sodium bisulfate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| GB1584703A true GB1584703A (en) | 1981-02-18 |
Family
ID=5977112
Family Applications (3)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB18660/77A Expired GB1584702A (en) | 1976-05-05 | 1977-05-04 | Process for the preparation of sodium bisulphate |
| GB38193/79A Expired GB1584703A (en) | 1976-05-05 | 1977-05-04 | Process for the preparation of sodium bisulphate granules |
| GB43993/79A Expired GB1584704A (en) | 1976-05-05 | 1977-05-04 | Process for the preparation of sodium bisulphate granules |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB18660/77A Expired GB1584702A (en) | 1976-05-05 | 1977-05-04 | Process for the preparation of sodium bisulphate |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB43993/79A Expired GB1584704A (en) | 1976-05-05 | 1977-05-04 | Process for the preparation of sodium bisulphate granules |
Country Status (6)
| Country | Link |
|---|---|
| JP (1) | JPS52133899A (en) |
| BE (1) | BE854299A (en) |
| DE (1) | DE2619811C2 (en) |
| FR (2) | FR2350302A1 (en) |
| GB (3) | GB1584702A (en) |
| IT (1) | IT1075526B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7067094B2 (en) * | 2003-09-09 | 2006-06-27 | Grillo-Werke Ag | Process for the brightening of sodium hydrogensulfate |
| CN102153111A (en) * | 2011-02-28 | 2011-08-17 | 绍兴市东湖生化有限公司 | Method for preparing anhydrous sodium hydrogen sulfate by using ethephon production waste liquid |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2810693C2 (en) * | 1978-03-11 | 1982-07-15 | Hoechst Ag, 6000 Frankfurt | Process for the continuous production of sodium bisulfate |
| CN116924344B (en) * | 2023-09-15 | 2023-11-17 | 潍坊石大昌盛能源科技有限公司 | Granulating method of sodium hydrosulfide |
-
1976
- 1976-05-05 DE DE2619811A patent/DE2619811C2/en not_active Expired
-
1977
- 1977-05-03 IT IT23136/77A patent/IT1075526B/en active
- 1977-05-04 GB GB18660/77A patent/GB1584702A/en not_active Expired
- 1977-05-04 JP JP5085677A patent/JPS52133899A/en active Pending
- 1977-05-04 GB GB38193/79A patent/GB1584703A/en not_active Expired
- 1977-05-04 GB GB43993/79A patent/GB1584704A/en not_active Expired
- 1977-05-05 BE BE177303A patent/BE854299A/en not_active IP Right Cessation
- 1977-05-05 FR FR7713684A patent/FR2350302A1/en active Granted
- 1977-11-09 FR FR7733729A patent/FR2392935A1/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7067094B2 (en) * | 2003-09-09 | 2006-06-27 | Grillo-Werke Ag | Process for the brightening of sodium hydrogensulfate |
| CN102153111A (en) * | 2011-02-28 | 2011-08-17 | 绍兴市东湖生化有限公司 | Method for preparing anhydrous sodium hydrogen sulfate by using ethephon production waste liquid |
Also Published As
| Publication number | Publication date |
|---|---|
| BE854299A (en) | 1977-11-07 |
| DE2619811C2 (en) | 1978-05-11 |
| GB1584702A (en) | 1981-02-18 |
| DE2619811B1 (en) | 1977-09-15 |
| GB1584704A (en) | 1981-02-18 |
| FR2350302A1 (en) | 1977-12-02 |
| FR2350302B1 (en) | 1983-01-14 |
| IT1075526B (en) | 1985-04-22 |
| FR2392935A1 (en) | 1978-12-29 |
| JPS52133899A (en) | 1977-11-09 |
| FR2392935B1 (en) | 1983-01-07 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PS | Patent sealed [section 19, patents act 1949] | ||
| PCNP | Patent ceased through non-payment of renewal fee |