US3888855A - Preparation of low bulk density sodium dichloroisocyanurate dihydrate - Google Patents

Preparation of low bulk density sodium dichloroisocyanurate dihydrate Download PDF

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US3888855A
US3888855A US378829A US37882973A US3888855A US 3888855 A US3888855 A US 3888855A US 378829 A US378829 A US 378829A US 37882973 A US37882973 A US 37882973A US 3888855 A US3888855 A US 3888855A
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bulk density
dihydrate
sodium dichloroisocyanurate
dichloroisocyanurate dihydrate
sodium
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US378829A
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Sidney Berkowitz
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Olin Corp
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FMC Corp
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Priority to AU69279/74A priority patent/AU482387B2/en
Priority to CA200,997A priority patent/CA1012969A/en
Priority to IT23652/74A priority patent/IT1014811B/en
Priority to NL7409041A priority patent/NL7409041A/en
Priority to FR7423414A priority patent/FR2241551B1/fr
Priority to BR5593/74A priority patent/BR7405593D0/en
Priority to DE2433113A priority patent/DE2433113C3/en
Priority to BE146448A priority patent/BE817516A/en
Priority to JP49078795A priority patent/JPS5037792A/ja
Priority to CH960574A priority patent/CH605852A5/xx
Priority to SE7409193A priority patent/SE420092B/en
Priority to ZA00744479A priority patent/ZA744479B/en
Priority to GB3087474A priority patent/GB1442503A/en
Priority to ES428242A priority patent/ES428242A1/en
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Assigned to OLIN CORPORATION, 120 LONG RIDGE ROAD, STAMFORD, CT. 06904, A CORP. OF VA. reassignment OLIN CORPORATION, 120 LONG RIDGE ROAD, STAMFORD, CT. 06904, A CORP. OF VA. ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: FMC CORPORATION, 2000 MARKET STREET, PHILADELPHIA, PA., A CORP. OF DE.
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
    • C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
    • C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
    • C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
    • C07D251/30—Only oxygen atoms
    • C07D251/36—Only oxygen atoms having halogen atoms directly attached to ring nitrogen atoms

Definitions

  • Dichloroisocyanurates are well-known materials which are widely used as a source of available chlorine in solid bleaching, sanitizing and detergent compositions.
  • the sodium and potassium salts are the most widely used in laundering compositions because they are very soluble and easily removed by rinsing.
  • the sodium dichloroisocyanurate compounds are known to exist in three forms, namely, the anhydrous form, the monohydrate (containing approximately 7.6% water of hydration by weight), and the dihydrate (containing approximately 141% water of hydration by weight). See Symes, US. Pat. Nos. 3,035,056 and 3,035,057.
  • One prior art procedure for producing sodium dichloroisocyanurate dihydrate involves the chlorination of trisodiumi socyanurate with gaseous chlorine.
  • the dihydrate solids produced by chlorination are separated from the bulk of the aqueous phase by wellknown methods for separating solids from liquids, and then dried to remove uncombined water to produce dry sodium dichloroisocyanurate.
  • Dihydrates produced in this manner have bulk densities of approximately 35 pounds/cubic foot or 0.56 grams/cubic centimeter. These dihydrates are effective as a source of available chlorine when mixed with components of solid bleaching and detergent compositions having the same bulk density.
  • Brown et al teach mixing a dichlorocyanurate (in acid or salt form) with a synergistic carrier agent mixture of sodium tripolyphosphate and sodium sulfate decahydrate. This mixture is heated and cooled to form a slurry or plastic mass, which is then dried at high temperatures, approximately 95C and pulverized to form a powdered product with a low bulk density whose water content can vary from 7 to 30%.
  • the bulk density of the final product is dependent upon the amount of water employed for combining the carrier agent and the dichlorocyanurate.
  • Moisture contents between and by weight form dense homogeneous products upon drying. As the moisture contents are increased up to 50% by weight, compositions of progressively decreasing bulk densities are produced upon drying.
  • the range of the bulk densities for the compositions produced in this manner are from 0.439 to 0.802 grams/cubic centimeter.
  • a storage-stable, free-flowing, thermal-decomposition resistant, low bulk density sodium dichloroisocyanurate dihydrate can be prepared from waterwet crystals of sodium dichloroisocyanurate dihydrate by contacting the water-wet dihydrate crystals with a water miscible organic solvent, then drying the solvent containing material at temperatures below about 48C to remove the contacting liquid and not the waters of hydration.
  • a sodium dichloroisocyanurate dihydrate product is produced having a bulk density at least four times lighter than sodium dichloroisocyanurate dihydrate prepared in the conventional manner.
  • low bulk density sodium dichloroisocyanurate dihydrate used to define the product of the invention means a sodium dichloroisocyanurate dihydrate having a bulk density of about 0.1 to about 0.3 grams/cubic centimeter.
  • Sodium dichloroisocyanurate dihydrate may be produced by any conventional manner and used in the process of the invention.
  • the dihydrate feed material may be in either dry or water-wet form.
  • dry dihydrate it is advantageous to dissolve the dry crystals in water in order to dissolve the crystalline agglomerates.
  • the solution containing the dissolved crystals is then evaporated and/or cooled, e.g. to below 12C, to reform the crystals.
  • the reformed crystals are then separated from the aqueous solution, mixed with the contacting liquid, and dried.
  • Precipitated sodium dichloroisocyanurate dihydrate produced by either conventional means or by dissolving crystalline agglomerates discussed above may be separated from the bulk of the aqueous reaction solution by any well-known means, such as by filtration, centrifugation, decantation or the like.
  • the treatment with the contacting liquid is carried out by adding the organic solvent to the precipitate and contacting and mixing the precipitate with the organic solvent.
  • the organic solvent should be added almost immediately to the separated precipitate to remove any residual reaction solution.
  • Such contacting results in the formation of low bulk density crystals which are approximately 3 X microns in size. If the mother liquor is allowed to remain on the crystals during separation, the crystals will break and agglomerate, resulting in crystals of higher bulk densities that are about 6 X 30 microns in size. If the precipitate is allowed to dry, it will cake in such a manner that complete contact with the solvent will be impossible.
  • the contacting liquid may be added completely at one time or added in small portions, each portion being drained completely before the next one is added. Generally, it is more efficient to employ two small portions of contacting liquid than one portion of the same total volume. When employing two or more portions of contacting liquid, the contacting liquid may be reused with fresh contacting liquid. Thorough mixing of the precipitate and contacting liquid is necessary if the full benefits of the invention are to be realized.
  • the contacting liquid used for contacting the waterwet dihydrate crystals must be an organic solvent that is miscible with water.
  • the boiling point of the solvent should be relatively low, that is less than about 48C, so that drying temperatures below about 48C will remove the solvent from the dihydrate but not the waters of hydration. If an organic solvent having a boiling point about 48C is desired, drying must be conducted under vacuum to assure drying at below 48C.
  • the solvent should also be chemically inert in the presence of the dihydrate. Examples of organic solvents which may be employed in my invention are acetone, methanol, tetrahydrofuran, and acetonitrile.
  • the dihydrate crystals After the dihydrate crystals have been thoroughly mixed with the contacting liquid, the dihydrate crystals are dried. Drying may be carried out by any known manner, such as by a warm air stream or in a vacuum oven.
  • Drying temperatures below about 48C are employed, and preferably between 25 and 35C. Temperatures slightly above 48C may be employed if losses of minor amountsof water of hydration can be tolerated. Temperaturesabove about 66C are avoided in order to prevent the formation of the anhydrous salt. Drying temperatures are employed which will remove the organic solvent retained by the precipitate but which will not remove the sodium diehloroisocyanurate waters of hydration.
  • the low bulk'density sodium diehloroisocyanurate crystals of the invention have an average size of 3 X 180 microns and a bulk density of about 0.1 to about 0.3 grams/cubic centimeter, preferably about 0.13 to about 0.25 grams/cubic centimeter. A particularly preferred bulk density is on the order of 0.13 grams/cubic centimeter.
  • Upon heating, both waters of hydration are lost in one step at temperatures between 48 and 66C.
  • These low bulk density crystals have the same excellent storage-stability and free-flowing properties as the conventionally prepared sodium diehloroisocyanurate dihydrate.
  • the inventive crystals are also resistant to thermal decomposition, a property which is an especial advantage of the dihydrate material.
  • EXAMPLE l-A Prior Art Preparation of Sodium Dichloroisocyanurate Dihydrate A by weight aqueous slurry of diehloroisocyanuric acid was prepared and fed into a reactor. A 50% sodium hydroxide solution was prepared and was simultaneously fed into the same reactor at a sufficient rate to maintain the pH at 6.8. The temperature of the reaction mixture was maintained between 20 and 25C by a water cooled heat exchanger. The resulting slurry containing precipitated sodium diehloroisocyanurate dihydrate was filtered through a medium porosity funnel to separate the salt from the aqueous medium. The separated salt was then gently dried at about 40C in a warm air stream for approximately 24 hours.
  • the resultant product was a free-flowing, white crystalline sodium diehloroisocyanurate dihydrate material. Available chlorine was assayed at 55.2%, theoretical 55.4%. The dihydrates bulk density was 35 pounds/cubic foot (0.56 grams/cubic centimeter).
  • EXAMPLE l-B Process of the Invention Sodium diehloroisocyanurate dihydrate was produced and recovered according to Example l except that no drying step was carried out. Immediately after filtration, the water-wet dihydrate crystals were thoroughly contacted and mixed with acetone. The acetone-wet salt product was then dried at about 30C in a warm air stream for approximately 24 hours. The resultant product was a fluffy, free-flowing, white crystalline product identified as sodium diehloroisocyanurate dihydrate material having an available chlorine assay of 55.2%; theoretical 55.4%. The dihydrate had a bulk density of 8.1 pounds/cubic foot (0.13 grams/cubic centimeter).
  • a process for the production of a storage-stable, free-flowing, thermal-decomposition resistant, low bulk density sodium diehloroisocyanurate dihydrate which comprises contacting water-wet sodium dichloroisocyanurate dihydrate with a water miscible organic solvent, drying the solvent treated sodium diehloroisocyanurate at a temperature less than about 48C to remove the organic solvent and not the waters of hydration, and recovering a low bulk density, sodium dichloroisocyanurate dihydrate having a bulk density of about 0.1 to about 0.3 grams/cubic centimeter.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Detergent Compositions (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

Process for producing a storage-stable, freeflowing, thermaldecomposition resistant, low bulk density sodium dichloroisocyanurate dihydrate by contacting a water-wet sodium dichloroisocyanurate dihydrate with a water miscible organic solvent and drying the solvent-wet material to remove the solvent from the material without removing the waters of hydration.

Description

United States Patent 1191 1111 3,888,855
Berkowitz June 10, 1975 PREPARATION OF LOW BULK DENSITY 3,035,057 5/1962 Symes 260/248 SODIUM DICHLOROISOCYANURATE 3,452,0l2 6/1969 Langenho'ff et al 260/248 DIHYDRATE 3,803,144 4/1974 Berkowitz 260/248 [75] Inventor: Sidney Berkowitz, Highland Park,
[73] Assignee: FMC Corporation, New York, NY.
[22] Filed: July 13, 1973 [21] Appl. N04 378,829
[52] US. Cl 260/248 C [51] Int. Cl C07d 55/38 [58] Field of Search 260/248 C [56] References Cited UNITED STATES PATENTS 3,035,056 5/1962 Symes 260/248 Primary ExaminerJ0hn M. Ford [5 7 ABSTRACT Process for producing a storage-stable, freeflowing, thermal-decomposition resistant, low bulk density sodium dichloroisocyanurate dihydrate by contacting a water-wet sodium dichloroisocyanurate dihydrate with a water miscible organic solvent and drying the solvent-wet material to remove the solvent from the material without removing the waters of hydration.
6 Claims, N0 Drawings PREPARATION OF LOW BULK DENSITY SODIUlVI DICHLOROISOCYANURATE DIHYDRATE This invention relates to the production of low bulk density sodium dichloroisocyanurate dihydrate from waterwet crystals of sodium dichloroisocyanurate dihydrate feed materials.
Dichloroisocyanurates are well-known materials which are widely used as a source of available chlorine in solid bleaching, sanitizing and detergent compositions. The sodium and potassium salts are the most widely used in laundering compositions because they are very soluble and easily removed by rinsing. The sodium dichloroisocyanurate compounds are known to exist in three forms, namely, the anhydrous form, the monohydrate (containing approximately 7.6% water of hydration by weight), and the dihydrate (containing approximately 141% water of hydration by weight). See Symes, US. Pat. Nos. 3,035,056 and 3,035,057.
One prior art procedure for producing sodium dichloroisocyanurate dihydrate involves the chlorination of trisodiumi socyanurate with gaseous chlorine. The dihydrate solids produced by chlorination are separated from the bulk of the aqueous phase by wellknown methods for separating solids from liquids, and then dried to remove uncombined water to produce dry sodium dichloroisocyanurate. Dihydrates produced in this manner have bulk densities of approximately 35 pounds/cubic foot or 0.56 grams/cubic centimeter. These dihydrates are effective as a source of available chlorine when mixed with components of solid bleaching and detergent compositions having the same bulk density. However, when admixed with components of a low bulk density or fluffy type bleaching or detergent formulation, uniform formulations are not obtained since the formulations segregate during storage or shipping. This segregation results in non-homogeneous formulations which do not yield consistent sanitizing and- /or bleaching action.
One attempt to produce preparations of bleaching, sterilizing and disinfecting compositions with varying bulk densities is disclosed by Brown et al in U.S. Pat. No. 3,293,188. Brown et al teach mixing a dichlorocyanurate (in acid or salt form) with a synergistic carrier agent mixture of sodium tripolyphosphate and sodium sulfate decahydrate. This mixture is heated and cooled to form a slurry or plastic mass, which is then dried at high temperatures, approximately 95C and pulverized to form a powdered product with a low bulk density whose water content can vary from 7 to 30%. The bulk density of the final product is dependent upon the amount of water employed for combining the carrier agent and the dichlorocyanurate. Moisture contents between and by weight form dense homogeneous products upon drying. As the moisture contents are increased up to 50% by weight, compositions of progressively decreasing bulk densities are produced upon drying. The range of the bulk densities for the compositions produced in this manner are from 0.439 to 0.802 grams/cubic centimeter.
Brown et als use of high temperatures (95C) to dry their compositions, results in decomposition of the dichloroisocyanurate and in a product wherein the sodium dichloroisocyanurate component must be in the anhydrous and/or the monohydrate form. Such decomposition also results in lowering availab'lechlorinecontent of the product. While the patentees state that their products are low bulk density materials, these products, when admixed with low bulk density or fluffy type bleaching or detergent formulations, become segregated during shipping and storage. Segregation results in formulations that fail to yield consistent sanitizing and/or bleaching action.
It is the object of my invention to produce a storagestable, free-flowing, thermal-decomposition resistant, low bulk density product without loss of available chlorine that will not cake, lump nor deliquesce when compounded and packaged, and which may be blended or admixed with low bulk density or fluffy type disinfecting, bleaching or detergent formulations.
I have discovered that a storage-stable, free-flowing, thermal-decomposition resistant, low bulk density sodium dichloroisocyanurate dihydrate can be prepared from waterwet crystals of sodium dichloroisocyanurate dihydrate by contacting the water-wet dihydrate crystals with a water miscible organic solvent, then drying the solvent containing material at temperatures below about 48C to remove the contacting liquid and not the waters of hydration. Quite unexpectedly, a sodium dichloroisocyanurate dihydrate product is produced having a bulk density at least four times lighter than sodium dichloroisocyanurate dihydrate prepared in the conventional manner.
The term low bulk density sodium dichloroisocyanurate dihydrate used to define the product of the invention means a sodium dichloroisocyanurate dihydrate having a bulk density of about 0.1 to about 0.3 grams/cubic centimeter.
Sodium dichloroisocyanurate dihydrate may be produced by any conventional manner and used in the process of the invention. The dihydrate feed material may be in either dry or water-wet form. When employing dry dihydrate, it is advantageous to dissolve the dry crystals in water in order to dissolve the crystalline agglomerates. The solution containing the dissolved crystals is then evaporated and/or cooled, e.g. to below 12C, to reform the crystals. The reformed crystals are then separated from the aqueous solution, mixed with the contacting liquid, and dried.
Precipitated sodium dichloroisocyanurate dihydrate produced by either conventional means or by dissolving crystalline agglomerates discussed above may be separated from the bulk of the aqueous reaction solution by any well-known means, such as by filtration, centrifugation, decantation or the like.
The treatment with the contacting liquid is carried out by adding the organic solvent to the precipitate and contacting and mixing the precipitate with the organic solvent. The organic solvent should be added almost immediately to the separated precipitate to remove any residual reaction solution. Such contacting, results in the formation of low bulk density crystals which are approximately 3 X microns in size. If the mother liquor is allowed to remain on the crystals during separation, the crystals will break and agglomerate, resulting in crystals of higher bulk densities that are about 6 X 30 microns in size. If the precipitate is allowed to dry, it will cake in such a manner that complete contact with the solvent will be impossible.
The contacting liquid may be added completely at one time or added in small portions, each portion being drained completely before the next one is added. Generally, it is more efficient to employ two small portions of contacting liquid than one portion of the same total volume. When employing two or more portions of contacting liquid, the contacting liquid may be reused with fresh contacting liquid. Thorough mixing of the precipitate and contacting liquid is necessary if the full benefits of the invention are to be realized.
The contacting liquid used for contacting the waterwet dihydrate crystals must be an organic solvent that is miscible with water. The boiling point of the solvent should be relatively low, that is less than about 48C, so that drying temperatures below about 48C will remove the solvent from the dihydrate but not the waters of hydration. If an organic solvent having a boiling point about 48C is desired, drying must be conducted under vacuum to assure drying at below 48C. The solvent should also be chemically inert in the presence of the dihydrate. Examples of organic solvents which may be employed in my invention are acetone, methanol, tetrahydrofuran, and acetonitrile.
After the dihydrate crystals have been thoroughly mixed with the contacting liquid, the dihydrate crystals are dried. Drying may be carried out by any known manner, such as by a warm air stream or in a vacuum oven.
Drying temperatures below about 48C are employed, and preferably between 25 and 35C. Temperatures slightly above 48C may be employed if losses of minor amountsof water of hydration can be tolerated. Temperaturesabove about 66C are avoided in order to prevent the formation of the anhydrous salt. Drying temperatures are employed which will remove the organic solvent retained by the precipitate but which will not remove the sodium diehloroisocyanurate waters of hydration.
The low bulk'density sodium diehloroisocyanurate crystals of the invention have an average size of 3 X 180 microns and a bulk density of about 0.1 to about 0.3 grams/cubic centimeter, preferably about 0.13 to about 0.25 grams/cubic centimeter. A particularly preferred bulk density is on the order of 0.13 grams/cubic centimeter. Upon heating, both waters of hydration are lost in one step at temperatures between 48 and 66C. These low bulk density crystals have the same excellent storage-stability and free-flowing properties as the conventionally prepared sodium diehloroisocyanurate dihydrate. The inventive crystals are also resistant to thermal decomposition, a property which is an especial advantage of the dihydrate material. Conventionally prepared sodium diehloroisocyanurate dihydrate crystals are in agglomerated form and have an approximate size of 6 X 30 microns and bulk densities above 0.56 grams/cubic centimeter. Upon heating, waters of hydration are released in two steps. The first water of hydration is removed at temperatures between 65 and 70C. The second water of hydration is removed at temperatures between 105 and 1 10C. 1
The following examples are given not by way of limitation, but merely as descriptive of the invention.
EXAMPLE l-A Prior Art Preparation of Sodium Dichloroisocyanurate Dihydrate A by weight aqueous slurry of diehloroisocyanuric acid was prepared and fed into a reactor. A 50% sodium hydroxide solution was prepared and was simultaneously fed into the same reactor at a sufficient rate to maintain the pH at 6.8. The temperature of the reaction mixture was maintained between 20 and 25C by a water cooled heat exchanger. The resulting slurry containing precipitated sodium diehloroisocyanurate dihydrate was filtered through a medium porosity funnel to separate the salt from the aqueous medium. The separated salt was then gently dried at about 40C in a warm air stream for approximately 24 hours. The resultant product was a free-flowing, white crystalline sodium diehloroisocyanurate dihydrate material. Available chlorine was assayed at 55.2%, theoretical 55.4%. The dihydrates bulk density was 35 pounds/cubic foot (0.56 grams/cubic centimeter).
EXAMPLE l-B Process of the Invention Sodium diehloroisocyanurate dihydrate was produced and recovered according to Example l except that no drying step was carried out. Immediately after filtration, the water-wet dihydrate crystals were thoroughly contacted and mixed with acetone. The acetone-wet salt product was then dried at about 30C in a warm air stream for approximately 24 hours. The resultant product was a fluffy, free-flowing, white crystalline product identified as sodium diehloroisocyanurate dihydrate material having an available chlorine assay of 55.2%; theoretical 55.4%. The dihydrate had a bulk density of 8.1 pounds/cubic foot (0.13 grams/cubic centimeter).
EXAMPLE 2 Horizontal Flame Propagation Test Samples from Examples l-A and l-B were tested according to Procedure Rl7593 of the US. Bureau of Mines. The samples were placed in a l X 2 X 7 inch bed and heated at one end with a propane torch. The rate of horizontal flame propagation was timed and measured. The products from Examples l-A and l-B showed no flame propagation and could not be ignited.
The invention being thus described, it will be obvious that the same may be varied in many ways. Such variations are not to be regarded as a departure from the spirit and scope of the invention, and all such modifications are intended to be included within the scope of the following claims.
What is claimed is:
1. A process for the production of a storage-stable, free-flowing, thermal-decomposition resistant, low bulk density sodium diehloroisocyanurate dihydrate which comprises contacting water-wet sodium dichloroisocyanurate dihydrate with a water miscible organic solvent, drying the solvent treated sodium diehloroisocyanurate at a temperature less than about 48C to remove the organic solvent and not the waters of hydration, and recovering a low bulk density, sodium dichloroisocyanurate dihydrate having a bulk density of about 0.1 to about 0.3 grams/cubic centimeter.
2. The process of claim 1 wherein the water miscible organic solvent is acetone.
3. The process of claim 2 wherein the drying temperature is between 25 and 35C.
4. Sodium diehloroisocyanurate dihydrate having a bulk density of about 0.1 to about 0.3 grams/cubic centimeter.
5.. Sodium diehloroisocyanurate dihydrate having a bulk density of about 0.13 to about 0.25 grams/cubic centimeter.
6. Sodium diehloroisocyanurate dihydrate having a bulk density of 0.13 grams/cubic centimeter.
UNITED STATES PATENT OFFICE CERTIFICATE OF CORRECTION PATENTNO. 3,888,855
DATED June 10, 1975 lNVENTOR(fi) Sidney Berkowitz It is certified that error appears in the above-identified patent and that said Letters Patent are hereby corrected as shown below:'
Abstract, line 1, "freeflowing" should read free-flow'ing-..
Column 1, line 6, "waterwet" should read --waterwet-.
Column 2, line 17, "waterwet" should read --water-wet-.
Column 3, line 13, "about" should read abo\ re--.
V Signed and Scaicd this eighth Day of June 1976 {SEAL} RUTH C. MASON C. MARSHALL DANN Arresting 0mm (mnmiuhmn ofParem: and Trademark:

Claims (5)

1. A PROCESS FOR THE PRODUCTION OF A STORAGE-STABLE, FREEFLOWING, THERMAL-DECOMPOSITION RESISTANT, LOW BULK DENSITY SODIUM DICHLOROISOCYANURATE DIHYDRATE WHICH COMPRISE CONSITACTING WATER-WET SODIUM DICHLOROISOCYANURATE DIHYDRATE WITH A WATER MISCIBLE ORGANIC SOLVENT, DRYING THE SOLVENT TREATED SODIUM DICHLOROISOCYANURATE AT A TEMPERTURE LESS THAN ABOUT 4(*C TO REMOVE THE ORGANIC SOLVENT AND NOT THE WATERS OF HYDRTION, AND RECOVERNG A LOW BULK DENSITY, SODIUM DICHLOROISOCYANURATE DIHYDRATE HAVING A BULK DENSITY OF ABOUT 0.1 TO ABOUT 0.3 GRMS/CUBIC CENTIMETER.
2. The process of claim 1 wherein the water miscible organic solvent is acetone.
3. The process of claim 2 wherein the drying temperature is between 25* and 35*C.
4. Sodium dichloroisocyanurate dihydrate having a bulk density of about 0.1 to about 0.3 grams/cubic centimeter. 5.. Sodium dichloroisocyanurate dihydrate having a bulk density of about 0.13 to about 0.25 grams/cubic centimeter.
6. Sodium dichloroisocyanurate dihydrate having a bulk density of 0.13 grams/cubic centimeter.
US378829A 1973-07-13 1973-07-13 Preparation of low bulk density sodium dichloroisocyanurate dihydrate Expired - Lifetime US3888855A (en)

Priority Applications (15)

Application Number Priority Date Filing Date Title
US378829A US3888855A (en) 1973-07-13 1973-07-13 Preparation of low bulk density sodium dichloroisocyanurate dihydrate
AU69279/74A AU482387B2 (en) 1974-05-23 Preparation of low bulk density sodium dichloroisocyanurate dihydrate
CA200,997A CA1012969A (en) 1973-07-13 1974-05-28 Preparation of low bulk density sodium dichloroisocyanurate dihydrate
IT23652/74A IT1014811B (en) 1973-07-13 1974-06-05 PREPARATION OF DICHLOROISOCYANURATE SODIUM BIHYDRATE OF LOW APPARENT DENSITY
NL7409041A NL7409041A (en) 1973-07-13 1974-07-04 PROCESS FOR THE PREPARATION OF LOW SHAKING WEIGHT SODIUM DICHLOROISOCYANURATE DIHYDRATE.
FR7423414A FR2241551B1 (en) 1973-07-13 1974-07-05
BR5593/74A BR7405593D0 (en) 1973-07-13 1974-07-08 PROCESS TO PRODUCE A LOW DENSITY SODIUM DIICHOROISOCIANURATE DIHYDRATE RESISTANT TO RESISTANT THERMAL DECOMPOSITION OF FREE AND STABLE FLOW DURING STORAGE
BE146448A BE817516A (en) 1973-07-13 1974-07-10 PROCESS FOR OBTAINING SODIUM DIHYDRATE DICHLOROISOCYANURATE WITH A LOW APPARENT SPECIFIC WEIGHT
DE2433113A DE2433113C3 (en) 1973-07-13 1974-07-10 Process for the preparation of dichloroisocyanurate dihydrate with a low bulk density
JP49078795A JPS5037792A (en) 1973-07-13 1974-07-11
CH960574A CH605852A5 (en) 1973-07-13 1974-07-11
SE7409193A SE420092B (en) 1973-07-13 1974-07-12 PROCEDURES FOR THE PREPARATION OF STORAGE STABLE, RELEASE, THROUGH THERMAL SUBSTITUTION RESISTANT LOW BULK DENSITY SODIUM CHLORISOCYANURATE DIHYDRATE
ZA00744479A ZA744479B (en) 1973-07-13 1974-07-12 Preparation of low bulk density sodium dichloroisocyanurate dihydrate
GB3087474A GB1442503A (en) 1973-07-13 1974-07-12 Preparation of low bulk density sodium dichloroisocyanurate dihydrate
ES428242A ES428242A1 (en) 1973-07-13 1974-07-13 Preparation of low bulk density sodium dichloroisocyanurate dihydrate

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FR (1) FR2241551B1 (en)
GB (1) GB1442503A (en)
IT (1) IT1014811B (en)
NL (1) NL7409041A (en)
SE (1) SE420092B (en)
ZA (1) ZA744479B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4182871A (en) * 1978-02-27 1980-01-08 Niro Atomizer A/S Process for spray drying sodium dichloroisocyanurate
US4503225A (en) * 1982-07-26 1985-03-05 Chemie Linz Aktiengesellschaft Process for the preparation of free-flowing, coarsely crystalline sodium dichloroisocyanurate dihydrate

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2486618C1 (en) * 2011-11-11 2013-06-27 Закрытое акционерное общество "Ультракрафт" Method of demagnetisation of ferromagnetic materials and device to this effect

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3035057A (en) * 1961-09-26 1962-05-15 Monsanto Chemicals Dichloroisocyanurate process and products
US3035056A (en) * 1962-05-15 Potassium dichloroisocyanurate
US3452012A (en) * 1965-11-09 1969-06-24 Dynamit Nobel Ag Process for the preparation of dry alkali dichlorisocyanurates
US3803144A (en) * 1972-05-15 1974-04-09 S Berkowitz Continuous production of sodium dichloroisocyanurate dihydrate

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3035056A (en) * 1962-05-15 Potassium dichloroisocyanurate
US3035057A (en) * 1961-09-26 1962-05-15 Monsanto Chemicals Dichloroisocyanurate process and products
US3452012A (en) * 1965-11-09 1969-06-24 Dynamit Nobel Ag Process for the preparation of dry alkali dichlorisocyanurates
US3803144A (en) * 1972-05-15 1974-04-09 S Berkowitz Continuous production of sodium dichloroisocyanurate dihydrate

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4182871A (en) * 1978-02-27 1980-01-08 Niro Atomizer A/S Process for spray drying sodium dichloroisocyanurate
US4503225A (en) * 1982-07-26 1985-03-05 Chemie Linz Aktiengesellschaft Process for the preparation of free-flowing, coarsely crystalline sodium dichloroisocyanurate dihydrate

Also Published As

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DE2433113C3 (en) 1979-12-06
DE2433113B2 (en) 1979-04-19
GB1442503A (en) 1976-07-14
DE2433113A1 (en) 1975-01-30
CH605852A5 (en) 1978-10-13
JPS5037792A (en) 1975-04-08
SE420092B (en) 1981-09-14
IT1014811B (en) 1977-04-30
NL7409041A (en) 1975-01-15
AU6927974A (en) 1975-11-27
BR7405593D0 (en) 1975-05-13
ZA744479B (en) 1975-07-30
ES428242A1 (en) 1976-07-16
FR2241551A1 (en) 1975-03-21
BE817516A (en) 1975-01-10
FR2241551B1 (en) 1978-11-24
SE7409193L (en) 1975-01-14
CA1012969A (en) 1977-06-28

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