DE1494906A1 - Process for producing a lead compound as a stabilizer for thermoplastic synthetic resins - Google Patents
Process for producing a lead compound as a stabilizer for thermoplastic synthetic resinsInfo
- Publication number
- DE1494906A1 DE1494906A1 DE19631494906 DE1494906A DE1494906A1 DE 1494906 A1 DE1494906 A1 DE 1494906A1 DE 19631494906 DE19631494906 DE 19631494906 DE 1494906 A DE1494906 A DE 1494906A DE 1494906 A1 DE1494906 A1 DE 1494906A1
- Authority
- DE
- Germany
- Prior art keywords
- lead compound
- stabilizer
- carboxylic acid
- plasticizer
- lead
- 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.)
- Withdrawn
Links
- 150000002611 lead compounds Chemical class 0.000 title claims description 10
- 239000003381 stabilizer Substances 0.000 title claims description 10
- 238000000034 method Methods 0.000 title claims description 9
- 229920003002 synthetic resin Polymers 0.000 title claims description 5
- 239000000057 synthetic resin Substances 0.000 title claims description 5
- 229920001169 thermoplastic Polymers 0.000 title claims description 5
- 239000004416 thermosoftening plastic Substances 0.000 title claims description 5
- 239000004014 plasticizer Substances 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 12
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 125000002837 carbocyclic group Chemical group 0.000 claims description 2
- 239000000470 constituent Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims 2
- 239000007900 aqueous suspension Substances 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 239000000428 dust Substances 0.000 description 5
- 235000021355 Stearic acid Nutrition 0.000 description 4
- 239000012065 filter cake Substances 0.000 description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 4
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000008117 stearic acid Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- BJQHLKABXJIVAM-UHFFFAOYSA-N Diethylhexyl phthalate Natural products CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- DJDSLBVSSOQSLW-UHFFFAOYSA-N mono(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(O)=O DJDSLBVSSOQSLW-UHFFFAOYSA-N 0.000 description 2
- 229920005992 thermoplastic resin Polymers 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000000080 wetting agent Substances 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910000004 White lead Inorganic materials 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 1
- PIJPYDMVFNTHIP-UHFFFAOYSA-L lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 description 1
- RYZCLUQMCYZBJQ-UHFFFAOYSA-H lead(2+);dicarbonate;dihydroxide Chemical compound [OH-].[OH-].[Pb+2].[Pb+2].[Pb+2].[O-]C([O-])=O.[O-]C([O-])=O RYZCLUQMCYZBJQ-UHFFFAOYSA-H 0.000 description 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N lead(II) oxide Inorganic materials [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 125000005608 naphthenic acid group Chemical group 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000003760 tallow Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/003—Compounds containing elements of Groups 4 or 14 of the Periodic Table without C-Metal linkages
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/14—Compounds of lead
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Paints Or Removers (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Description
PATENTANWALTPATENT ADVOCATE
. .. 8MÜNCHEN2. .. 8MUNICH2
An dieTo the
TAL 18VAL 18
Bundespatentbehörden RUF: 08ii/i947 98Federal Patent Authorities RUF: 08ii / 1947 98
8 München 2 * 28 . 7 · 196;) II/m8 Munich 2 * 28. 7 · 196;) II / m
Aktenzeichen ρ ^i4 94 9θ6.5 Λ File number ρ ^ i 4 94 9θ6.5 Λ
Anmelder: Associated Lead Manufacturers Limited, London, GroßbritannienApplicant: Associated Lead Manufacturers Limited, London, Great Britain
Verfahren zum Herstellen einer Bleiverbindung als Stabilisator für thermoplastische KunstharzeMethod of making a lead connection as a stabilizer for thermoplastic synthetic resins
Die Erfindung betrifft ein Verfahren zum Herstellen einer pulverförmigen anorganischen Bleiverbindung ais Stabilisator für thermoplastische Kunstharze, wobei die Pulver- λ partikel unter Verwendung einer organischen Carbonsäure durch einen dünnen Überzug eines flüssigen Weichmachers staubfrei gemacht werden.The invention relates to a method for manufacturing a powdery inorganic lead compound ais stabilizer for thermoplastic resins, wherein said powder λ particles using an organic carboxylic acid by a thin coating of a liquid plasticizer to be made free of dust.
Verschiedene Bleiverbindungen werden als Stabilisatoren für thermoplastische Kunstharze, z.B. Polyvinylchlorid, verwendet. Typische Beispiele solcher Bleiverbindungen sind basisches Bleisulfat, zweibasisches Bleiphosphid, basisches Bleikarbonat, basisches Bleisilikat. Es ist bekannt, diese Stabilisatoren dem Harz in Pastenform zuzugeben, wobei diese Paste normalerweise 5-7 Gewichtsteile des Stabilisators und 1 Gewichtsteil des Weichmachers enthält. Ein solcher Stabilisator ist jedoch nicht anwendbarVarious lead compounds are used as stabilizers used for thermoplastic synthetic resins such as polyvinyl chloride. Typical examples of such lead compounds are basic lead sulfate, dibasic lead phosphide, basic lead carbonate, basic lead silicate. It is known, add these stabilizers to the resin in paste form, this paste normally 5-7 parts by weight of the stabilizer and 1 part by weight of the plasticizer. However, such a stabilizer is not applicable
909883/1647909883/1647
U9A906U9A906
wenn aus dem Harz feste Körper, wie z.U. tlohre, hergestellt werden sollen, in denen jeder hohe Weichmaohergehait nachteilig ist. Deshalb wurde der Stabilisator dem Harz in Form eines trockenen Pulvers beigegeben. Solche Pulver neigen jedoch zu starker Staubbildung, was der Gesundheit der damit beschäftigten Arbeiter schadet.if solid bodies from the resin, e.g. tlohre, made should be, in which everyone has a high level of softness is disadvantageous. Therefore, the stabilizer was added to the resin in the form of a dry powder. However, such powders tend to generate a lot of dust, which is harmful to the health of the workers involved.
Ein Viertel des festen Filterkachengewichtes macht der Weichmacheranteil auch aus, wenn ein das Hleisalz enthaltender Filterkuchen mit einem Weichmacher behandelt wird, um eine Dispersion des Bleisalzes im Weichmacher zu erhalten, wozu ein aus einer gesättigten monobasisohen Carbonsäure mit 6 - Ib C-Atomen bestehendes Netzmittel verwendet wird (brit. Patentschrift 798 h'ik) . Wird ein Netzmittel nicht verwendet (brit. Patentschrift 7'i« 675) , dann liegt der Weichmacheranteil bei einem Drittel des fes ten Filterkuchengewichtes.A quarter of the solid filter cake weight is also made up of plasticizer when a filter cake containing the lead salt is treated with a plasticizer in order to obtain a dispersion of the lead salt in the plasticizer, for which purpose a wetting agent consisting of a saturated monobasic carboxylic acid with 6 lb carbon atoms is used (British Patent 798 h'ik) . If a wetting agent is not used (British patent specification 7'i «675), the plasticizer content is one third of the solid filter cake weight.
Um diese Nachteile zu vermeiden, ist es die Aufgabe der Erfindung, eine pulverförmig Bleiverbindung mit einem gleichmäßigen Überzug eines flüssigen Weichmachers herzusteilen, so daü mit dem so behandelten Puder ohneStaubentwicklung gearbeitet werden kann, während andererseits so wenig Weichmacher zugegeben wird, daü die mechanischen Eigenschaften des stabilisierten Harzes nicht nachteilig beeinflußt werden.In order to avoid these disadvantages, it is the object of the invention to provide a powdery lead compound with a to produce a uniform coating of a liquid plasticizer, so there with the powder treated in this way without creating dust can be worked, while on the other hand so little plasticizer is added that the mechanical Properties of the stabilized resin are not adversely affected.
Die Erfindung sieht zur Lösung dieser Aufgabe ein Verfahren vor, das dadurch gekennzeichnet ist, daü eine wässrige Suspension des Pulvers der Bleiverbindung mit einer Lösung des flüssigen Weichmachers und einer organischen Carbonsäure, die ein wasserunlösliches Bleisalz bildet, versetzt wird und hierauf die suspendierten Bestandteile in bekannter Weise durch Filtern abgeschieden, getrocknet und wieder pulverisiert werden.To achieve this object, the invention provides a method which is characterized in that it is an aqueous one Suspension of the powder of the lead compound with a solution of the liquid plasticizer and an organic one Carboxylic acid, which forms a water-insoluble lead salt, is added and then the suspended constituents deposited in a known manner by filtering, dried and pulverized again.
909883/1647909883/1647
H94906H94906
-J--J-
Vorteilhaft wird eine carbocyclische Säure verwendet. Typische. Beispiele sind die n-hexoic Säure, Dodecansiiure (Laurinsäure), Stearinsäure, Mischungen, die Stearinsäure enthalten, wie z.B. hydrierte fettige Talgsäuren, Iiensosiiure, Phthalsäure und Mischungen der Carbonsäuren, die aus Petroleum gewonnen wurden und allgemein als Naphthensäuren bekannt sind.A carbocyclic acid is advantageously used. Typical. Examples are the n-hexoic acid, dodecanoic acid (lauric acid), stearic acid, mixtures containing stearic acid contain, such as hydrogenated fatty tallow acids, eniosoic acid, phthalic acid and mixtures of carboxylic acids, derived from petroleum and commonly known as naphthenic acids.
Jeder normalerweise zur Gewinnung thermoplastischer Harzverbindungen benutzte Weichmacher kann verwendet werden, ^ z.B. Mineralöl, Ester der Phthalsäure und Ester der Adipinsäure.Any normally for the production of thermoplastic resin compounds Used plasticizers can be used, e.g. mineral oil, esters of phthalic acid and esters of Adipic acid.
Nachdem die suspendierten Feststoffe mit der Weiehraacher-Carbonsäuremischung in Reaktion gegangen sind, wird die überschüssige Wassermenge durch Filtern oder andere passende Mittel entfernt. Der Filterkuchen wird dann getrocknet, vorzugsweise bei einer Temperatur von nicht mehr als ilo C und der getrocknete Kuchen wird dann zer- ■ drückt und pulverisiert.After the suspended solids with the Weiehraacher carboxylic acid mixture have gone into reaction, the excess amount of water is filtered or other appropriate Funds removed. The filter cake is then dried, preferably at a temperature of not more than ilo C and the dried cake is then crushed ■ and pulverized.
Normalerweise wird die Menge des benutzten WeichmachersUsually the amount of plasticizer used will be
zwischen 0,5 und 8 Gewichtsprozent des Pulvers und die i between 0.5 and 8 percent by weight of the powder and the i
Menge der Carbonsäure zwischen 0,1 und 2 Gewichtsprozent des Pulvers schwanken.Amount of carboxylic acid vary between 0.1 and 2 percent by weight of the powder.
Nachfolgend sind Beispiele des erfindungsgemäßen Verfahrens aufgeführt:Below are examples of the method of the invention listed:
0,58 kg Bleiglätte wurden unter dauerndem Rühren in 27 1 Wasser dispergiert, wozu dann 6,β 1 80#ige Essigsäure und schließlich 8O kg 77#ige Schwefelsäure hinzugefügt wurden.0.58 kg of black lead were dispersed in 27 l of water with constant stirring, then 6, β 1 80% acetic acid and finally 80 kg of 77% sulfuric acid were added became.
U9A906U9A906
Nachdem die Reaktion zwischen der Bleiglätte und der Schwefelsäure beendet war, wurde eine Lösung von 4,53 kg Stearinsäure in 19 kg von 2-Äthyl-Hexyl-Phthalat zu der Suspension unter dauerndem Rühren hinzugegeben. Die suspendierte Masse wurde dann durch Filtern abgeschieden und der sich ergebende Kuchen bei einer Temperatur von lüü°C in einem Ofen getrocknet.After the reaction between the black lead and the sulfuric acid ended, a solution of 4.53 kg of stearic acid became in 19 kg of 2-ethyl hexyl phthalate to the Added suspension with constant stirring. The suspended mass was then separated out by filtering and drying the resulting cake at a temperature of 10 ° C in an oven.
Der getrocknete Kuchen wurde dann zerstoßen und gemahlen, " um ein Pulver zu erhalten, das im Falle des Aufwühlens keinen Staub entwickelt.The dried cake was then crushed and ground "to give a powder that in case of churning." no dust developed.
Bei diesem Beispiel waren die Mengen der Bleiglätte, der Essigsäure und der Schwefelsäure die gleichen wie in Beispiel i. Nachdem die Reaktion zwischen der Bleiglätte und der Schwefelsäure vollzogen war, wurde zu der Suspension eine Losung von 2,5 kg Stearinsäure in 9,4 kg 2-Athyl-Hexyl-Phthaiat unter dauerndem Rühren hinzugefügt. Die suspendierte Masse wurde durch Filtern getremt und getrocKnet, zerstoilen und gemahlen wie in Beispiel 1. Das P getrocknete und gemahlene Material ergab ein Pulver, das keinerlei Staub bildet.In this example, the amounts of litharge, acetic acid and sulfuric acid were the same as in FIG Example i. After the reaction between the black lead and the sulfuric acid was complete, it became the suspension a solution of 2.5 kg of stearic acid in 9.4 kg of 2-ethylhexyl phthalate added while stirring continuously. The suspended mass was separated by filtering and dried, crushed and ground as in Example 1. The P dried and ground material gave a powder which does not form any dust.
Die Erfindung umfaßt also einen Stabilisator für thermoplastisches Kunstharz, der aus einer pulverförraigen Bleiverbindung mit einem gleichmäßigen Überzug eines flussigen Weichmachers gemäß dem oben beschriebenen Verfahren besteht. The invention thus comprises a stabilizer for thermoplastics Synthetic resin, which consists of a powdery lead compound with an even coating of a liquid Plasticizer according to the method described above.
909883/ 1647909883/1647
Claims (3)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEA0043213 | 1963-05-29 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| DE1494906A1 true DE1494906A1 (en) | 1970-01-15 |
| DE1494906B2 DE1494906B2 (en) | 1970-12-17 |
Family
ID=6933528
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE19631494906 Withdrawn DE1494906B2 (en) | 1963-05-29 | 1963-05-29 | Process for producing a lead compound as a stabilizer for thermoplastic synthetic resins |
Country Status (4)
| Country | Link |
|---|---|
| BE (1) | BE630809A (en) |
| DE (1) | DE1494906B2 (en) |
| GB (1) | GB967084A (en) |
| NL (1) | NL294239A (en) |
-
0
- BE BE630809D patent/BE630809A/xx unknown
- NL NL294239D patent/NL294239A/xx unknown
-
1961
- 1961-11-10 GB GB4038061A patent/GB967084A/en not_active Expired
-
1963
- 1963-05-29 DE DE19631494906 patent/DE1494906B2/en not_active Withdrawn
Also Published As
| Publication number | Publication date |
|---|---|
| DE1494906B2 (en) | 1970-12-17 |
| BE630809A (en) | |
| NL294239A (en) | |
| GB967084A (en) | 1964-08-19 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| E77 | Valid patent as to the heymanns-index 1977 | ||
| EHJ | Ceased/non-payment of the annual fee |