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ARMED SERVICES TECHNICAL INFORMATION AGENCYARLINGTON HALL STATIONARLINGTON 12, VIRGINIA

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NOTICE: When government or other drawings, speci-fications or other data are used for any purposeother than in connection with a definitely relatedgovernment procurement operation, the U. S.Government thereby incurs no responsibility, nor anyobligation whatsoever; and the fact that the Govern-ment may have formulated, furnished, or in any waysupplied the said drawings, specifications, or otherdata is not to be regarded by implication or other-wise as in any manner licensing the holder or anyother person or corporation, or conveying any rightsor permission to manufacture, use or sell anypatented invention that may in any way be relatedthereto.

I 3!

TMR 1901

DESIN SUDYON A ALERNTE MTHO FO

PRODUCTION~ OF&~4 AMMONIU PECLRT -

17~i. Jul 196

U.- S. NA A PR P LL N PLANT,

IN IA EA , A YL N

TMR 190

17 July 1961

DESIGN STUDY ON AN ALTERNATE METHOD FORPRODUCTION OF AMMONIUM PERCHLORATE (U)

by

J. E. Dodgen

U. S. NAVAL PROPELLANT PLANTIndian Head, Maryland

0. A. WESCHE J. E. DODGENCaptain, USNavy Commander, USNRCommanding Officer Technical Director

TMR 190

FOREWORD

The study presented here was completed in mid-1958. There--fore, the price information is somewhate out of date, but a quickreview of current information indicates that changes in cost ofingredients and byproducts are favorable to the proposed process.

J. E. Dodgen

Technical Director

Released by:

0. A. WESCHECaptain, USNavyCommanding Officer

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TMR 190

CONTENTS

Heading: Page no.

Foreword iiiAbstract viProposed Alternate Process 1Advantages 7Manufacturing Costs 8Target Price 10Reference 11

FIGURE

1. Flow Chart for the Production of AmmoniumPerchlorate (10 T/Day) 3

TMR 190

ABSTRACT

Preparation of ammonium perchlorate by double decompo-sition of ammonium sulfate and sodium perchlorate was used todetermine a target price for economic production.

vi

TMR 190

DESIGN STUDY ON AN ALTERNATE METHOD FORPRODUCTION OF AMMONIUM PERCHLORATE

The increased importance of ammonium perchlorateas a component of missile propellants makes it advisable to reviewthe techniques of manufacture not only to establish alternate sourcesbut also to establish a reasonable economic target price. This reportincludea a design study and cost estimates for preparation of ammo-nium perchlorate by a double decomposition reaction between sodiumperchlorate and ammonium sulfate. The electrolytic process forproduction of sodium perchlorate from sodium chlorate offers littleopportunity for improvement.

In the most widely used commercial process, sodium perchlorateis reacted with ammonia and hydrochloric acid and the ammonium per-chlorate and sodium chloride are then removed by fractional crystalliza-tion. This process has several disadvantages:

(1) The hot chloride solution in the presence of oxidizerscauses excessive stress corrosion cracking and general corrosion ofthe process vessels;

(2) Problems in metering the hydrochloric acid and ammoniamake it difficult to maintain optimum pH;

(3) Variation in pH makes it necessary to recycle as much as20% to 40% of the product before it will meet specifications.

The ammonium perchlorate produced in this type of operation costsfrom $0.34 to $0.40 per pound.

PROPOSED ALTERNATE PROCESS

The double decomposition reaction between ammonium sulfateand sodium perchlorate was selected for study because of the wide-spread availability of ammonium sulfate. Furthermore, informationis available on the equilibria of solutions resulting from this reaction.Freeth(1 ) showed ammonium perchlorate and sodium sulfate can beprepared by reacting equivalent weights of sodium perchlorate andammonium sulfate In a mother liquor consisting of either.

TMR 190

Sodium sulfate can then be recrystallized from the hot and ammo-nium perchlorate from the cold remainder.

Equipment required includes a sodium perchlorate-ammoniumsulfate dissolver, sodium sulfate vacuum crystallizer, and ammo-nium perchlorate cooling crystallizer. Solids feeders for the dissolverand a centrifuge and dryer for each crystallizer are also required.Figure 1 is a flow chart for a 10-ton-per-day ammonium perchlorateplant showing equipment, flow rates, and compositions. This designcan be scaled directly.

Ammonium sulfate and sodium perchlorate are added to thedissolver which is maintained at 650 C to ensure solution of the reac-tants in the recycled mother liquor. The effluent passes to thesodium sulfate crystallizer. By application of heat and constantvacuum, process water is removed and the sodium sulfate is crystal-lized. Sodium sulfate is then removed in a slurry from the suspen-sion container of the crystallizer, dewatered, washed, and dried. Theeffluent at 60' C passes to the ammonium perchlorate crystallizer.After the solution has been cooled to 250 C, ammonium perchlorateis selectively crystallized. The product is then dewatered, washed,and dried. Mother liquor from the ammonium perchlorate crystallizeris returned to the dissolver for reuse.

Material Balance

Based on a closed-cycle continuous process, the followingliquor concentrations were selected:

Dissolver Sodium sulfate Ammonium perchlorateeffluent (%) crystallizer crystallizer effluent(%)

effluent.( %) stallizereffluent__)Na 2SO 4 23.4 18.4 20.6NH 4ClO 4 15.1 16.1 6.0(NH 4)2 SO 4 10.0 10.7 12.0H2P 51.5 54.8 61.4

The material balance is based on the following equation:

132.14 2(122.45) 2(117.50) 142.05(NH 4 )2 804 + 2NaClO4 - 2NH 4C10 4 + Na2 SO 4

NH4ClO 4 - 1OT/day- 834 lb/hr- 13. 9 lb/min

2

p TMR 190

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Na 2SO4 - 6.04 T/day-- 503 lb/hr-8.38 lb/min

(NH 4) 2SO4 - 5.62 T/day- 468 lb/hr- 7.8 lb/min

NaC1O 4 - 10.42 T/day- 868 lb/hr- 14.4 lb/min

The flow rates were determined from the solution compositions toprovide a production rate of 10 T/day ammonium perchlorate.

(NH 4)280 4 to dissolver 7. 8 lb/min at STPNaC10 4 to dissolver 14.4 lb/min at STPMother liquor to dissolver 115. 7 lb/min at 25V CSolution to Na2 SO4 crystallizer 137. 9 lb/min at 65° CSolution to NH 4C10 4 crystallizer 129. 6 lb/min at 60* CNa 2 SO4 produced 8. 38 lb/minNH4 C10 4 produced 13. 9 lb/min

Heat Balance

The heat balance for this process was accomplished by takingeach unit in this closed system and analyzing the heat involved.Assumptions were made as to the specific heat of the solutions, radia-tion and convection losses, and heat required to evaporate waterintroduced as centrifuge wash.

Dissolver:

The heat balance on the dissolver is based on taking 115. 7 lb/minof mother liquor at 250 C and heating to 650 C and concurrently dis-solving 7.8 lb/min of ammonium sulfate and 14.4 lb/min of sodiumperchlorate. The resulting solution of 137 9 lb/mln at 65° C is sentto the sodium sulfate crystallizer.

Heat of Reaction: The standard heat of reaction at 25' C wascalculated for the following reaction:

(NH 4)2SO4 (c) -2NaCIO 4(c)-% -2NH 4C1O4 (sotu) + Na2SO4(SOIU)

4

TMR 190

(NH4)2S0 4(c)AH =-; = -13,500 CHU (7.8 lb)

2NaClO4(Q)AH = -Qf = -24,600 CHU (14. 4 lb)

2NH4C1O4 (solu)AH= -Qf = -18,500 CHU (13.9 lb)

Na2SO4(solu)AH= -Qf = -19, 800 CHU (8.4 lb)

-13, 500 -24,600 = -18, 500 -19 800 + QR

QR = 200 CHU

Heat of reaction = 360 BTU/min

Sensible Heat: Heat required to raise temperature of solution,including reactant, from 770 F to 1490 F (At = 720 F).

Qs = wcpAt

Qs = 137.9 lb/min x 0.75 x 720 F

QS = 7447 BTU/min

Heat Loss- In order to estimate the heat loss it is necessaryto establish the approximate size of the dissolver. Sodium sulfatehas an inverted solubility. In order to prevent salting out on theheater surface, the maximum temperature rise should not be morethan 10-30 F. This would require a circulating system of about600-700 gpm with the dissolver holding about 2000 gal. With about250 sq ft of surface and 2 in. of insulation, the heat loss is estimated.

R X 2/12 =

KA 0. 0418 x 250 0.016_ t 90

t -R - 0. 016 -5625 BTUJ/hr

Heat Requirements (dissolver).

Qf= Q +RS + Q1Q = 360 - 7447 - 93Q = -7180 BTU/min

= - 430,800 BTU/hr

Sodium Sulfate Crystallizer.

The heat balance on this crystallizer is based on introducing137. 9 lb/min of solution at 650 C, supersaturating the solution by

5

TMR 190

vacuum evaporation and cooling the solution to 60V C. Sodium sulfatewill be crystallized at the rate of 8. 38 lb/min. The overflow of thecrystallizer, 129.6 lb/ min at 600 C, passes to the ammonium per-chlorate crystallizer. In addition to the heat of crystallization andsensible heat in the feed solution, the heat losses of radiation andconvection and heat required to evaporate excess process water areconsidered.

Heat of Crystallization:

Qc H W -358 8.38=CM- 142.005

Qc = -21 CHU

Qc= -38 BTU/min

Sensible Heat:

QS = CpW t

= 0.75 x 137.9 lb/min x 5 x 1.8= 931 BTU/min

Heat Loss: is assumed to be twice as large as it is in thedissolver since vapor body and suspension container are involved.

Q, = 186 BTU/min

Process Water Evaporation: It is assumed that about 5 lb/minof water will be required to be evaporated. This amount will beintroduced through centrifuge washer and pump seals.

Qe =Hw =1100 x 5

Qe = 5, 500 BTU/min

Heat Requirements: (Na 2SO4 Crystallizer)

Q = QC + QS + Q1 + Qe

Q = -38 + 931 - 186 - 5500

Q = -4793 BTU//min

Ammonium Perchlorate Crystallizer:

The heat requirements for this crystallizer are based on taking129.6 lb/min of liquor at 600 C, cooling this liquor in the crystallizer

6

TMIRf 190

to 25° C, and crystallizing ammonium percblorate. The balance of

115. 7 lb/min of mother liquor at 250 C will be returned to the dissolver.

Heat of Crystallization:w 13.__9

Qc = HOE'= 6360 x 137.9

Mij=3O 117.5c= 752 CHU

Qc = 1354 BTU/min

Sensible Heat:

Qs CfWA0.N75 x 129. 6 x 35 x 1. 8

= 6124 BTU/min

Heat Loss: Heat loss at 25° C is negligible.

Total Heat:

Q= Qc+QSQ = 1354 + 6124Q = 7478 BTU/min

ADVANTAGES

The process proposed here will simplify the selection ofmaterials of construction and the maintenance of equipment.Rubber-lined tanks for hydrochloric acid, pressure storage tanksfor ammonia, and high-vacuum equipment for ammonium per-chlorate crystallization will not be necessary. The glass-linedreactor required for addition of ammonia and hydrochloric acidwill also not be necessary.

With the proposed process, a standard 304 or 316 stainlesssteel should be adequate. From the standpoint of economic con-siderations and plant layout, further refinements in the processmight be made. The water used to dissolve the sodium perchloratefor transport to the processing area might be eliminated; themother liquor might be substituted for the water but this has somedisadvantages.

7

MANUFACTURING COSTS

The purpose of this section is to discuss the cost of ammoniumperchlorate. By analysis of the market costs of various chemicalsused in the existing, proposed, and related processes, the expected

p •manufacturing costs have been determined.

"Basic Cost:

These data are based on prices taken from Hi-Lo ChemicalPrice Issue of the Oil, Paint, and Drug Reporter.

Chemical Price/lb Price/tonSodium chlorate $0.09Potassium chlorate 0.1125Potassium chloride 0. 014 $28Sodium chloride 0.005 10Potassium perchlorate 0.1850Ammonia 0.036 72Muriatic acid (200 Be) 0.015 30Sodium sulfate 0.026 52Ammonium sulfate 0. 021 42

Processing Cost:

The object of this part is to determine the processing costfor converting a salt by double decomposition reaction accompaniedby crystallization. The following reaction was selected as typicalof this type of process:

0.871b 0.611b 0.481b llbNaClOs + KCI - NaCI + KCIO3

Processing cost is determined by subtracting the credit for sodiumchloride produced from the ingredient cost and, in turn, subtractingthis ingredient cost figure from the cost of the product.

NaC1O 3 = 0.87 x . 09 = 0.0783KC] =0.61 x.014 =0.0085

0. 0868NaCl =0.48 x.005 =0.0024

0. 0844KC1O3 =1 x.1125 =0.1125

- 0. 0844Processing Cost 0. 0281

8

TMR 190

Therefore, the processing cost in this type of process is estimatedto be about $0.03 per pound of product.

Sodium Perchlorate:

This chemical is not an article of trade. No published priceexists. It is necessary to estimate the cost for sodium perchlorateby using the following process:

0.891b 0. 541b -- s 0. 421b llbNaC10 4 + KCI NaC1 + KC104

By using the processing cost previously determined, the cost ofsodium perchlorate is determined.

Processing cost = 0.0300KC1 = 0.54 x.014 = 0.0076

0.0376

Less NaC1 credit (0.42 x .005 ) 0.0021Ingredient and process cost 0.0355

KC104 = 1 x.1850 = 0.1850Less ingredients and processing = 0. 0355NaC10 4 (0.89 lb) 0.1495

= 0.1680/lb

Therefore, sodium perchlorate Is estimated at a unit cost of$0.1680 per pound. Considering that sodium chlorate costs $0. 09 perpound, the spread of about $0.08 per pound of sodium perchlorateis adequate to allow converting sodium chlorate to sodium perchlorate.

Proposed Process:

The cost of ammonium perchlorate produced by the proposedprocess would be as follows:

0.56 lb 1.04 lb - 0.60 lb I lb(NH 4)2SO 4 + 2NaC1O 4 Na 2SO 4 + 2NH4C10 4

(NH4)2SO4= 0. 56 x 0. 021 = 0.0118NaCIO4 = 1.04 x 0. 1680 = 0. 1747Processing = 0. 0300

0.2165Less Na280 4 credit 0.0159NH4C10 4 cost 0.2006

9

TMR 190

Existing Process:

A comparable cost for manufacture of ammonium perchlorateby an existing process is shown as follows:

0.311b 0.141b 1. 0411b 0.51b llbHCI + NH3 + NaCl0 4 -- NaCi + NH4CIO4

Il 1HCl = 0.31 x 1 x 0. 015 =.0148

.3145NHs = 0.14 x .036 = .0054NaClO 4 = 1. 04 x. 1680 =. 1747Processing = 0300

.2249Less NaCi credit = . 0025NH 4C10 4 cost .2224

TARGET PRICE

The proposed process is about $0. 022 per pound less expen-sive than the existing process. Therefore, the real target pricefor ammonium perchlorate is about $0. 20 per pound. This repre-sents a potential saving to the government of $0. 14 to $0.20 perpound.based on the current price of $0. 34 to $0.40 per pound.On the basis of 1, 000, 000 pounds per month, this amounts to anannual saving of from $1, 680) 000 to $2, 400, 000 per year, The costinvolved in obtaining a specific particle size distribution has notbeen considered.

10

TMR 190

REFERENCE

(1) F. A. Freeth. "Ternary and Quaternary Equilibra in the System:Sodium Perchlorate-Ammonium Sulfate-Ammonlum Perchlorate-Sodium Sulfate-Water at 600 and 250. Rec. Tray. Chim.Vol. 43:475-507 (1924).

11

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