KR100493348B1 - Sized Paper and Its Use in High Speed Converting or Reprographics Operations - Google Patents

Abstract

The present invention comprises the steps of sizing paper under alkaline conditions with alkenyl succinic anhydride (ASA) and 2-oxetanone but not solid at 35 ° C., and using the paper for high speed processing or electronic radiation operations. The present invention relates to a method of using paper for high speed processing or electronic copying. The present invention also provides a paper under alkaline conditions comprising providing a sizing agent comprising alkenyl succinic anhydride (ASA) and 2-oxetanone that is not solid at 35 ° C., and sizing the paper with the sizing agent. It relates to a method of manufacturing.

Description

Sized paper and its use in High Speed Converting or Reprographics Operations}

The present invention relates to a method of using alkaline sized paper for high speed processing or electronic copying operations.

Fine papers manufactured under alkaline conditions can reduce costs, use precipitated calcium carbonate, and there is an increasing desire to improve the durability and whiteness of paper, and the wet end of paper machines The amount increased rapidly due to the increasing tendency not to use.

When using many current high land, special attention is required to sizing before processing or final use. Examples include high speed copy paper, envelopes, forms bonds and adder paper including computer printer paper. The most common sizing agents for algae prepared under alkaline conditions are alkenyl succinic anhydride (ASA) and alkyl ketene dimer (AKD). They both have reactive functionalities that are believed to covalently bond with cellulose fibers and hydrophobic tails oriented outward from the fibers. Due to the nature and orientation of these hydrophobic tails, the fibers push out the water.

Commercial AKDs containing one β-lactone ring (also known as 2-oxetanone ring) are prepared from the two most widely used, straight-chain fatty acid chlorides made from palmitic and / or stearic acid. Prepared by dimerization of alkyl ketenes. Other ketene dimers, such as alkenyl-based ketene dimers (Aquapel 421 available from Hercules Incorporated, Wilmington, Delaware, USA), have also been used commercially.

Commercially available ASA-based sizing agents are prepared by the reaction of maleic anhydride with olefins containing from about 14 to about 22 carbon atoms.

Although ASA and AKD sizing agents are commercially successful, they have disadvantages. On paper machines, ASA often forms deposits, which can break the paper web and even puncture the paper. If the level of ASA added to the paper is greater than 2.0 to 2.5 lb / ton, paper runner performance is generally unacceptable and the quality of the paper is problematic. However, it is often necessary to size 2.0 to 2.5 lb / ton or more for sizing paper made using a large amount of filler. Finally, the ASA cannot be shipped and stored in emulsion form for extended periods of time, so the papermaker must make the emulsion just before use.

For AKD-based sizing agents, the most frequently mentioned problem is the sizing speed on the paper machine. Often the curing time has to be extended before the sizing is complete.

These two types of sizing agents, particularly AKD, cause handling problems in the high speed machining operations typically required when using advanced papers (hereinafter referred to as alkali advanced papers) manufactured under alkaline conditions. Such problems include reduced work speeds in forms presses and other processing machines, double feeds or jams in high-speed copiers, and locations in high-speed printing and envelope-folding devices. Registration errors, etc. In recent years, non-solid 2-oxetanone sizing agents have been introduced at 35 ° C. to solve handling problems in high-speed machining operations (e.g., pre- commercially available from Hercules Incorporated, Delaware, USA). Precis 2000).

One of the issues of handling in such high speed machining operations is "Improving the Converting and End Use Performance of Alkaline Fine Paper", TAPPI 1994 Paper Makers Conference Proceedings, Book 1 (1994), 155-163. Page]. This problem occurs when using the IBM 3800 High Speed Continuous Form Laser Printer, which has not been specially modified to facilitate handling of alkaline deposits. Therefore, this commercially important laser printer can serve as an effective testing device for determining the processability in state-of-the-art processing equipment of various types of sized paper and its subsequent end use performance. In particular, the "billowing" phenomenon allows the IBM 3800 printer to measure the amount of slippage between an inoperative roll over the fuser and a driven roll on the stacker. Indicates.

This billing problem deviates from the straight line between the rolls and is two inches (5 cm) above the base plate, causing alignment errors and dropped folds in the stacker. The blowdown speed during steady-state running time is multiplied by 10000 by the blowing height (inches) over a straight paper path after 600 seconds of run time.

When the sizing agent addition level is higher than 2.2 lb / ton (1 kg / 0.9 metric ton paper), typical alkaline AKD sized papers typically exhibit an unacceptable degree of blown rate of 20 to 80. Paper handling speeds on Hamilton-Stevens continuous foam presses or other high speed processing machines such as the Winkler & Dunnebier CH envelope folders are also a numerical measure of machinability.

EP 0 629 741 A1 discloses a paper sized with 2-oxetanone sizing agent which is a mixture of 2-oxetanone multimers and alkyl ketene dimers of various molecular weights. This paper exhibits sizing levels comparable to paper sized with current alkyl ketene dimers and alkenyl succinic anhydride sizing agents, and exhibits improved performance in high speed processing and electronic copiers.

U.S. Patent 5,685,815 and European Patent Application 0 666 368 disclose papers that are sized with a 2-oxetanone sizing agent and do not exhibit machine feeding problems in high speed processing or electronic copying machines. This 2-oxetanone sizing agent is prepared from fatty acids that are liquid at temperatures below 35 ° C. and have structural irregularities on hydrocarbon chains, such as carbon-carbon double bonds or chain branches.

U. S. Patent No. 5,725, 731 discloses papermaking sizing compositions that do not cause machine feed problems in high speed processing. This sizing composition comprises a mixture of 2-oxetanone compounds that are not solid at 35 ° C. and are the reaction product of a mixture of saturated fatty acids and unsaturated fatty acids.

US Pat. No. 5,407,537 teaches the use of synthetic reactive sizing compounds that eliminate the need for emulsifiers and reduce hydrolysis of the sizing compounds while in process water. Preferred synthetic reactive sizing compounds are alkenyl succinic anhydrides having alkenyl groups having 8 to 16 carbon atoms. The possibility of using mixtures of alkenyl succinic anhydrides with alkyl ketene dimers is also described.

British patent application GB 2,252,984 A discloses a sizing composition which is a blend of 3 to 50 wt% alkyl ketene dimer and 97 to 50 wt% alkyl or alkenyl cyclic acid anhydride.

 Swedish patent application 893,906 discloses a packaging board for a fluid sized with a combination of alkyl ketene dimer and alkenyl succinic anhydride.

The alkyl ketene dimers disclosed in US Pat. No. 5,407,537, UK patent application GB 2,252,984 A and Swedish patent application 893,906 are solid alkyl ketene dimers.

There is a need for alkali deposits that provide improved handling in typical processing and electronic radiation operations. At the same time, the sizing level should be achieved to be comparable to the current level of alkali upper 2-oxetanone or ASA.

<Overview of invention>

The present invention comprises the steps of sizing paper under alkaline conditions with alkenyl succinic anhydride (ASA) and 2-oxetanone but not solid at 35 ° C., and using the paper for high speed processing or electronic radiation operations. The present invention relates to a method of using paper for high speed processing or electronic copying. Preferably, the 2-oxetanone sizing agent comprises at least one 2-oxetanone compound that is the reaction product of a reaction mixture comprising an unsaturated monocarboxylic fatty acid, wherein the term "fatty acid" is conveniently referred to as a fatty acid or fatty acid halide. It means.

 In another embodiment, the present invention comprises providing a sizing agent comprising alkenyl succinic anhydride (ASA) and 2-oxetanone that is not solid at 35 ° C., and sizing the paper with the sizing agent And a method for producing paper under alkaline conditions.

1 and 2 show a blend of (a) 2-oxetanone that is not solid at 35 ° C., (b) alkenyl succinic anhydride (ASA) and (c) ASA and 2-oxetanone that is not solid at 35 ° C. It is a graph showing the natural aged sizing level obtained when added several times.

In the following description, the term "fatty acid" is intended to mean fatty acids or fatty acid halides for convenience. Those skilled in the art will refer to the fatty acids used in the process of making the sizing composition herein, since fatty acids are converted into acid halides, preferably chlorides, in the first step of preparing the 2-oxetanone compound. It will be appreciated that the present invention can be practiced with, as starting materials, fatty acids or fatty acids already converted to acid halides. Moreover, those skilled in the art generally mean "fatty acid" to mean a pure fatty acid or fatty acid halide, or because a fatty acid is usually a blend or mixture as it is derived from natural acid, it may also mean a blend or mixture of fatty acids or fatty acid halides. You will know.

2-oxetanones of the present invention are disclosed in US Pat. Nos. 5,685,815 and 5,725,731. 2-oxetanone, which may be a blend of 2-oxetanone, is not a solid at 35 ° C. (it is not substantially a crystalline, semi-crystalline or waxy solid, ie they do not give heat of fusion upon heating and are fluid). Preferably, 2-oxetanone is not solid at 25 ° C, and more preferably is not solid at 20 ° C. Even more preferably, 2-oxetanone is a liquid at 35 ° C., more preferably a liquid at 25 ° C., and most preferably a liquid at 20 ° C.

2-oxetanone according to the invention is a mixture of compounds of the general formula:

Wherein n is preferably 0 to 6, more preferably 0 to 3, most preferably 0; R and R "are the same or different and are saturated or unsaturated, straight or branched, alkyl groups of 8 to 24 carbon atoms; R 'is saturated or unsaturated, straight or branched, 2 to 40 An alkyl group consisting of 4, preferably 4 to 32 carbon atoms; at least 25% of the R and R ″ groups in the mixture of compounds are unsaturated.

2-oxetanone may comprise a mixture of 2-oxetanone compounds that are the reaction products of a reaction mixture comprising an unsaturated monocarboxylic fatty acid. The reaction mixture may further comprise saturated monocarboxylic fatty acids and dicarboxylic acids.

Preferably, the reaction mixture used to prepare the mixture of 2-oxetanone compounds comprises at least 25% by weight unsaturated monocarboxylic fatty acids, more preferably at least 70% by weight unsaturated monocarboxylic fatty acids.

The unsaturated monocarboxylic fatty acid included in the reaction mixture used for the preparation of the 2-oxetanone compound is preferably 10 to 26, more preferably 14 to 22, most preferably 16 to 18 carbons. Contains an atom Examples of such acids include, for example, oleic acid, linoleic acid, dodecenoic acid, tetradecenoic acid (myristoleic acid), hexadecenoic acid (palmitoleic acid), octadecadenoic acid (linolelideic acid), and octadecatriene. Acids (linolenic acid), eicosane acid (gadoleic acid), eicosaterateic acid (arachidonic acid), cis-13-dococenic acid (erusic acid), trans-13-dococenic acid (brasidic acid), and docosapenta Enic acid (clophanodonic acid) and its halides, preferably chlorides. One or more such monocarboxylic fatty acids may be used. Preferred unsaturated monocarboxylic fatty acids are oleic acid, linoleic acid, linolenic acid and palmitoleic acid and acid halides thereof. Most preferred unsaturated monocarboxylic fatty acids are oleic acid and linoleic acid, and acid halides thereof.

The saturated monocarboxylic fatty acid used to prepare the 2-oxetanone compound for use in the present invention is preferably 10 to 26, more preferably 14 to 22, most preferably 16 to 18 carbons. Contains an atom Examples of such acids include stearic acid, isostearic acid, myristic acid, palmitic acid, margaric acid, pentadecanoic acid, decanoic acid, undecanoic acid, dodecanoic acid, tridecanoic acid, nonadecanoic acid, arachidic acid and beech. Henic acid, and halides thereof, preferably chloride. One or more of these saturated monocarboxylic fatty acids may be used. Preferred acids are palmitic acid and stearic acid.

The alkyl dicarboxylic acid used in the preparation of the 2-oxetanone compound used in the present invention preferably contains 6 to 44, more preferably 9 or 10, 22 or 36 carbon atoms. Examples of such dicarboxylic acids include sebacic acid, aselaic acid, 1,10-dodecandioic acid, suveric acid, brazilian, docosanedic acid, and C ₃₆ dimeric acids, for example, Ohio, USA EMPOL 1008 commercially available from Henkel-Emery, Cincinnati, and its halides, preferably chlorides. One or more of the dicarboxylic acids may be used. More preferred are dicarboxylic acids having 9 or 10 carbon atoms. Most preferred dicarboxylic acids are sebacic acid and azelaic acid.

When dicarboxylic acid is used in the preparation of 2-oxetanone for use in the present invention, the maximum molar ratio of dicarboxylic acid to monocarboxylic acid (including both saturated and unsaturated) is preferably about 5. More preferred maximum molar ratio is about 4, and most preferred maximum molar ratio is about 2.

Mixtures of 2-oxetanone compounds can be prepared using known methods of preparing standard ketene dimers. In the first step, acid halides, preferably acid chlorides, are prepared from mixtures of fatty acids or mixtures of fatty acids and dicarboxylic acids, using PCl ₃ or other halogenating agents, preferably chlorinating agents. The acid halide is then converted to ketene in the presence of a tertiary amine (including trialkyl amines and cyclic alkyl amines), preferably triethylamine. The ketene residues are then dimerized to form 2-oxetanone.

Alkenyl succinic anhydrides (ASA) blended with 2-oxetanone in the present invention are described by CEFarley and RBWasser, which are incorporated herein by reference. Edition ", published by WF Reynolds, Tappi Press, 1989, pages 51-62. ASA consists of an unsaturated hydrocarbon chain containing pendant succinic anhydride groups. Preferred liquid ASAs in the process of the invention are typically prepared by a two step process with alpha olefins as starting material. First the olefin isomerizes by moving the double bond randomly from the alpha position. In the second step, the isomerized olefin is reacted with excess maleic anhydride to the final ASA structure as shown in the reaction scheme below.

If the isomerization step is omitted, ASA can be prepared that is a solid at room temperature.

The alpha olefin starting material preferably has 14 to 22 carbon atoms and can be linear or branched. For the purposes of the present invention, it is more preferred that ASA is prepared by the reaction of maleic anhydride with olefins containing 14 to 18 carbon atoms. Typical structures found in ASA are disclosed in US Pat. No. 4,040,900, which is incorporated herein by reference.

A variety of ASAs are available from Albemarle Corporation, Baton Lauge, Louisiana.

Representative olefin starting materials to be reacted with maleic anhydride to prepare ASA for use in the present invention include octadecene, tetradecene, hexadecene, eicodecene, 2-n-hexyl-1-octene, 2-n- Octyl-1-dodecene, 2-n-octyl-1-decene, 2-n-dodecyl-1-octene, 2-n-octyl-1-octene, 2-n-octyl-1-nonene, 2- n-hexyl-1-decene and 2-n-heptyl-1-octene.

In the blend of ASA and 2-oxetanone, the maximum molar ratio of 2-oxetanone to ASA is preferably about 9: 1. More preferably the maximum molar ratio is about 4: 1, most preferably about 2: 1. The minimum molar ratio of 2-oxetanone to ASA is preferably about 1: 9. More preferably, the minimum molar ratio is about 1: 4, most preferably the minimum molar ratio is about 1: 2.

Generally, the sizing agents of the present invention are used in the form of dispersions or emulsions, which can be prepared by methods known in the art. The sizing agent is preferably used as an internal sizing agent, that is, it is preferably added to the paper pulp slurry before sheet formation. ASA and 2-oxetanone sizing components may be preblended or added separately prior to addition.

The paper of the present invention preferably has a total sizing agent of at least 0.5 lb (0.2 kg), more preferably at least about 1.5 lb (0.8 kg) and most preferably at least about 2.2 lb / ton (1 kg / 0.9 metric ton) (Ie a mixture of ASA and 2-oxetanone) are sized as addition levels. The paper of the present invention may be in the form of, for example, continuous foam bond paper, perforated continuous foam paper, adder paper, or envelope paper, as well as processed products such as copy paper and envelopes.

Preferably the alkaline paper produced according to the process of the invention contains a water soluble inorganic salt of an alkali metal, preferably sodium chloride (NaCl). However, the paper of the present invention is often made without NaCl.

The use of the paper of the present invention in high speed processing or electronic copying operations has several advantages over the use of paper sized only with ASA or 2-oxetanone but not solid at 35 ° C. First, when the level of addition is medium to low, the paper of the present invention is naturally aged sizing (after 7 days of aging at room temperature) compared to paper sized with the same amount of 2-oxetanone but not solid at 35 ° C. Sizing level is higher. Secondly, the paper of the present invention produces mechanical deposits at lower levels than when sized with the same amount of ASA sizing agent. Third, on-machine sizing is better when using a mixture of ASA and non-solid 2-oxetanone at 35 ° C. than using only non-solid 2-oxetanone at 35 ° C. This is often important for the running on paper machines.

Moreover, the process of the present invention is also advantageous over the case of sizing paper using ASA and a solid alkyl ketene dimer. If solid alkyl ketene dimers are used, a special apparatus is necessary for melting the alkyl ketene dimers to prepare an aqueous dispersion. This melting step is not necessary in the case of liquid 2-oxetanone.

The paper of the present invention does not cause significant machine-feeding problems in high speed processing machines or electronic copying operations. In particular, the paper according to the present invention has a basis weight of about 15 to 24 lb / 1300 ft ² (6.8 to 10.9 kg / 121 m ² ), the sizing agent addition level is about 1.5 lb / ton (0.68 kg / 0.9 metric ton), It can then be manufactured as a roll of continuous foam bond paper, which can run on the IBM Model 3800 high speed continuous form laser printer without causing significant machine feeding problems.

Furthermore, preferred according to the present invention, which can be prepared as a sheet of cutting paper for 8.5 × 11 inch (21.6 cm × 28 cm) copying having a basis weight of about 15 to 24 lb / 1300 ft ² (6.8 to 10.9 kg / 121 m ² ). Paper can travel on high speed laser printers or copiers. Paper adds at least about 1.5 lb / ton (0.68 kg / 0.9 metric ton), more preferably at least about 2.2 lb / ton (1 kg / 0.9 metric ton) total sizing agent (ie a mixture of ASA and 2-oxetanone) When sized to the level, the paper can run on an IBM Model 3825 high-speed copier at speeds of at least 5 of 10000 sheets, preferably of 1 or less of 10,000 sheets, without causing intermediate feeding or paper jams. In comparison, paper sized with standard AKD has a much larger double feed rate on the IBM 3825 high-speed copier (14 out of 14250 double feeds). In normal copier operation, a dual feed of 10 of 10000 sheets is unacceptable. Machine manufacturers say that a double supply of one out of 10,000 is acceptable.

The paper of the present invention in the form of a roll of continuous foam bond paper having a basis weight of about 15 to 24 lb / 1300 ft ² (6.8 to 10.9 kg / 121 m ² ), at a press speed of about 1300 to 2000 ft (390 m to 600 m) / min or more It can be converted to a standard perforated continuous foam on a continuous foam press. Bone in the form of a roll of continuous foam bond paper having a basis weight of about 15 to 24 lb / 1300 ft ² (6.8 to 10.9 kg / 121 m ² ) and sized to an addition level of about 2.2 lb / ton (1 kg / 0.9 metric ton) or greater Preferred papers of the invention can be converted to standard perforated continuous foam on a Hamilton-Stevens continuous foam press at a press speed of at least about 1775 ft (541 m) / min, preferably at least about 1900 ft (579 m) / min.

The paper of the present invention is a roll of envelope paper having a basis weight of about 15 to 24 lb / 1300 ft ² (6.8 to 10.9 kg / 121 m ² ) and sized to an addition level of about 2.2 lb / ton (1 kg / 0.9 metric ton) or more. It can also be made. The paper may be converted into an envelope of at least about 900 sheets per minute, preferably at least about 1000 sheets per minute, on a Winkler and Dunnevir CH envelope folding machine.

The paper of the present invention can travel on a high speed sheet-fed copier (IBM 3825) at a speed of about 58 sheets / min or more with a double feed rate or paper jam rate of less than one in 10,000 sheets.

The paper of the present invention is a paper in the form of a roll of continuous form bond paper on a high speed continuous form laser printer, having the same basis weight as the paper of the present invention and sized to the same level with an AKD sizing agent prepared from a mixture of stearic acid and palmitic acid. When traveling on the same printer, after 10 minutes of travel time, it is possible to travel with a billing speed of at least about 10% less, preferably at least about 20%.

The paper of the present invention is placed on a high speed sheet-feeding copier (IBM 3825) with the same basis weight as the paper of the present invention and the same copier with a paper sheet sized to the same level with an AKD sizing agent made from a mixture of stearic and palmitic acid. With a double feed rate or paper jam rate of at least about 50% less than the double feed rate or double jam rate when traveling above, preferably about 70%, it can travel at a speed of about 58 sheets / min.

The paper of the present invention also has a press rate of at least 3% greater than a paper sized at the same level with an AKD sizing agent prepared from a mixture of stearic acid and palmitic acid with the same basis weight as the paper of the invention It can be converted to standard perforated continuous foams on continuous foam presses at high press speeds.

Experimental Process

All parts, percentages, etc. herein are by weight unless otherwise indicated.

Paper for evaluation on the IBM 3800 was made on a pilot paper machine. To make the paper stock of a typical foam bond paper, a double disk refiner was used to add pulp furnish (3 parts southern hard kraft pulp and 1 part southern soft kraft pulp) to 425 ml Canada. Refined to Canadian Standard Freeness (CSF). Before adding the filler to the pulp furnish (10% medium particle size precipitated calcium carbonate), the pH, alkalinity and hardness of the paper stock are adjusted to pH 7.8 to 8.0 using an appropriate amount of H ₂ SO ₄ , NaHCO ₃ , NaOH and CaCl ₂ . The alkalinity was adjusted to 150 to 200 ppm and the hardness to 100 ppm.

2-oxetanone compounds were prepared using methods commonly used to make commercial 2-oxetanone compounds. That is, an acid chloride is made from a mixture of fatty acids using a conventional chlorinating agent, which is then dehydrochlorinated in the presence of a suitable base. ASA is alkenyl succinic anhydride C16C18, purchased from Albemal Corporation, Baton Lauge, Louisiana, USA.

An emulsion of ASA / 2-oxetanone blends, cited herein by C. Y. Paley and Al B. Wasser, "The Sizing of Paper, Second Edition", published by WF Reynolds, Tappi Press, 1989, 51-62 Prepared immediately before use by the method described in [Page]. Uses Starok 400 cationic starch (available from AEStaley Manufacturing Co., Decatur, Ill.) With a starch to sizing agent ratio of 3: 1. To prepare an emulsion.

Sizing agent, quaternary-amine-substituted cationic starch (0.75% for Example 3, 0.5% for Examples 1 and 2), alum (0.2%) and retention aid (0.025%) Wet end was added. The paper stock temperature in the headbox and white water tray was adjusted to 110 ° F (43.3 ° C).

The wet press was set to a 40 psi (2.8 kg / cm 2) gauge. A dryer was used that provided 1-2% moisture in the sizing press and 4-6% moisture in the reel (77 ft (23.4 m) / min). Stayco C (oxidized corn starch) (A Starley Manufacturing Co., Decatur, Ill.) About 35 lb / ton (15.9 kg / 0.9 metric ton), and NaCl 1 lb / ton ( 0.45 kg / 0.9 metric ton) was added to the sizing press (130 ° F. (54.4 ° C.), pH 8). Calender pressure and reel moisture were adjusted so that the Sheffield smoothness on the reel (column 2, face up of paper) was 150 flow units.

The paper roll for 35 minutes was collected and processed on a commercial foam press to obtain two boxes of standard 8.5 "x 11" (21.6 x 28 cm) form. Samples were also collected before and after each 35 minutes to test natural aging sizing, base weight (46 lb / 3000 ft ² , 20.8 kg / 279 m ² ), and smoothness.

The processed paper was equilibrated in the printer room for at least one day before evaluation. Each paper box was evaluated on an IBM 3800 for 10-14 minutes (220 ft (66.7 m) / min). All samples were tested twice. To restore the initial mechanical conditions, standard acidic grades were run for at least 2 minutes between each assessment.

To evaluate whether the sizing agent is causing difficulties in the machining operation, the paper was produced in a pilot paper machine, processed and printed on an IBM 3800 high speed printer. Runability on the IBM 3800 was used as a measure of machinability. In particular, the processability was evaluated using the height (inches) and billing speeds in which the paper was blown between two defined rolls of IBM 3800. The faster and higher the sheet is blown, the worse the workability.

The Hercules Sizing Test (HST) is an industry standard test that measures the degree of sizing. This method uses an aqueous dye solution as a penetrant to optically detect the tip of the liquid moving through the sheet. The device determines the time taken for the reflectance of the sheet surface not in contact with the penetrant to drop to a predetermined percentage of the original reflectance. Unless otherwise stated, all recorded HST test data were measured in seconds for 80% reflectance with 1% formic acid ink mixed with naphthol Green B dye. The test using formic acid ink is a more severe test than the test using neutral ink, and the test time tends to be shorter. Higher HST values are better than lower ones.

<Example 1>

In this example, sizing efficiency at several sizing agent addition levels was evaluated for a 1: 1 blend of 2-oxetanone and alkenyl succinic anhydride. For comparison, a 2-oxetanone alone sample and an ASA alone sample were run under the same conditions.

2-oxetanone was prepared by a conventional process using Emersol-221 as feedstock. Emersol-221, available from Henkel-Emery, Cincinnati, Ohio, has a composition of 75% oleic acid, 8% linoleic acid, 6% palmitoleic acid, 3% myristoleic acid, 1% linolenic acid, and 9% saturated fatty acids.

ASA is an alkenyl succinic anhydride C16C18, purchased from Albemal Corporation, Baton Lauge, Louisiana, USA.

The evaluation data is shown in Table 1 below and graphically shown in FIG. 1. The data show that at the same level of sizing agent addition, the natural aging sizing efficiency by the ASA / 2-oxetanone blend is worse than that by ASA alone, but better than that by 2-oxetanone alone.

Experiment Sizing agent Sizing Agent Level (lb / ton Dry Paper) Natural Aging Sizing Efficiency (HST) (sec) 1A (comparative) 2-oxetanone 1.5 2 1B (comparative) 2-oxetanone 2.25 82 1C (comparative) 2-oxetanone 3.0 143 1D (comparative) ASA 1.1 34 1E (comparative) ASA 1.4 153 1F (comparative) ASA 1.7 186 1G 1: 1 2-oxetanone / ASA 1.4 41 1H 1: 1 2-oxetanone / ASA 1.8 116 1I 1: 1 2-oxetanone / ASA 2.25 194

<Example 2>

In this example, sizing efficiency at several sizing agent addition levels was evaluated for two ratios of 2-oxetanone and alkenyl succinic anhydride blends. For comparison, a 2-oxetanone alone sample and an ASA alone sample were run under the same conditions.

2-oxetanone and ASA were the same as those used in Example 1.

The results are shown in Table 2 below and graphically shown in FIG. 2. The data shows that the natural aging sizing efficiency when the 2-oxetanone / ASA ratio is 3: 1 and 65:35 is worse than with ASA alone when the addition level is less than about 2.75 lb / ton, and 2-jade It can be seen that it is better than that with the setanone alone.

Experiment Sizing agent Sizing Agent Level (lb / ton Dry Paper) Natural Aging Sizing Efficiency (HST) (sec) 2A (comparative) 2-oxetanone 1.5 2 2B (comparative) 2-oxetanone 2.25 50 2C (comparative) 2-oxetanone 3.0 289 2D (comparative) ASA 1.1 34 2E (comparative) ASA 1.4 178 2F (comparative) ASA 1.7 226 2G 3: 1 2-oxetanone / ASA 1.5 14 2H 3: 1 2-oxetanone / ASA 2.25 128 2I 3: 1 2-oxetanone / ASA 3.0 217 2J 65:35 2-oxetanone / ASA 1.5 13 2K 65:35 2-oxetanone / ASA 2.25 165 2L 65:35 2-oxetanone / ASA 3.0 223

<Example 3>

In this example, the effects of three ratios of 2-oxetanone and alkenyl succinic anhydride blends on the runability of alkali grades of difficult grade in the IBM 3800 were evaluated. Comparative Experiment 3A uses Hercon 70 sizing agent, a dispersion containing an alkyl ketene dimer prepared from a mixture of palmitic and stearic acid available from Hercules Incorporated, Wilmington, Delaware, USA. It was. The material used in the remaining experiments was as described in Example 1.

The evaluation results are shown in Table 3. This data shows that the paper sized by all three ratios of 2-oxetanone / ASA blends tested runs on the IBM 3800 with good to very good runability. Furthermore, at the addition level of 3.0 lb / ton, all three proportions of paper tested with the sizing agent tested run better on the IBM 3800 than papers sized only with Hercon 70.

Experiment Sizing agent Sizing Agent Level (lb / ton Dry Paper) IBM 3800 Machinability ^* 3A (comparative) Hercon 70 3.0 2.5 3B 1: 1 2-oxetanone / ASA 3.0 2 3C 1: 3 2-oxetanone / ASA 3.0 1.5 3D 3: 1 2-oxetanone / ASA 3.0 One * IBM runability 1-Very good (blowing speed × 10 ⁴ <2.1 in / sec) 2-Excellent (blowing speed × 10 ⁴ = 2.1-6.2 in / sec) 3-Bad (blowing speed × 10 ⁴ = 6.2 -16.7 in / sec) 4-Very bad (blowing rate × 10 ⁴ => 16.7 in / sec)

The examples given herein illustrate the specific embodiments of the present invention without restricting it. Various modifications and variations can be made in the present invention without departing from the scope of the appended claims.

Claims (30)

Sizing the paper under alkaline conditions with alkenyl succinic anhydride (ASA) and 2-oxetanone but not solid at 35 ° C., and using the paper for high-speed processing or electronic copying operations. Use for high speed machining or electronic copying. 2. The process of claim 1, wherein said 2-oxetanone comprises at least one 2-oxetanone compound that is a reaction product of a reaction mixture comprising an unsaturated monocarboxylic fatty acid. 3. The process of claim 2 wherein said reaction mixture comprises at least 25% by weight unsaturated monocarboxylic fatty acid. 4. The process of claim 3, wherein said reaction mixture comprises at least 70% by weight unsaturated monocarboxylic fatty acids. The unsaturated monocarboxylic fatty acid according to any one of claims 2 to 4, wherein the unsaturated monocarboxylic fatty acid is oleic acid, linoleic acid, dodecenoic acid, tetradecenoic acid (myristoleic acid), hexadecenoic acid (palmitoleic acid), octadecadiic acid (li) Nooleic acid), octadecatenic acid (linolenic acid), eicosane acid (gadoleic acid), eicosaterateic acid (arachidonic acid), cis-13-docosenoic acid (erusic acid), trans-13-dococenic acid ( Brasidic acid), and at least one fatty acid selected from the group consisting of docosapentaenoic acid (clopanodonic acid) and their acid halides. 6. The method of claim 5 wherein said unsaturated monocarboxylic fatty acid comprises at least one fatty acid selected from the group consisting of oleic acid, linoleic acid, linolenic acid and palmitoleic acid, and their acid halides. The process according to claim 2, wherein the reaction mixture comprises at least 25% by weight of oleic acid or acid halide thereof. 8. The process of claim 7, wherein said reaction mixture comprises at least 70% by weight of oleic acid or acid halide thereof. The process of claim 2, wherein the reaction mixture comprises at least 25% by weight of linoleic acid or acid halides thereof.  10. The process of claim 9, wherein the reaction mixture comprises at least 70% by weight of linoleic acid or acid halides thereof. The method of claim 1, wherein the 2-oxetanone is not solid at 25 ° C. 6. The method of claim 1, wherein the 2-oxetanone is a liquid at 25 ° C. 6. 13. The method of claim 12, wherein said 2-oxetanone is a liquid at 20 ° C. The process of claim 2, wherein the reaction mixture further comprises saturated monocarboxylic fatty acid. The method of claim 14, wherein the saturated monocarboxylic fatty acid is stearic acid, isostearic acid, myristic acid, palmitic acid, margaric acid, pentadecanoic acid, decanoic acid, undecanoic acid, dodecanoic acid, tridecanoic acid, nonadecane A method comprising at least one fatty acid selected from the group consisting of acids, arachidic acid and behenic acid, and their acid halides. 15. The method of claim 14, wherein said saturated monocarboxylic fatty acid comprises palmitic acid or stearic acid or their acid halides. The process of claim 2, wherein the reaction mixture further comprises a dicarboxylic acid or acid halide thereof. 6. The process of claim 5 wherein said dicarboxylic acid comprises dicarboxylic acid containing 8 to 36 carbon atoms. The process according to claim 1, wherein the ASA is the reaction product of maleic anhydride and an olefin having 14 to 18 carbon atoms. The method of claim 19, wherein the ASA is octadecene, tetradecene, hexadecene, eicodecene, 2-n-hexyl-1-octene, 2-n-octyl-1-dodecene, 2-n-octyl-1- Decene, 2-n-dodecyl-1-octene, 2-n-octyl-1-octene, 2-n-octyl-1-nonene, 2-n-hexyl-1-decene and 2-n-heptyl-1 -A reaction product of olefins selected from the group consisting of octenes and maleic anhydride. 5. The method of claim 1, wherein the ratio of 2-oxetanone to ASA is about 9: 1 or less. 6. The method of claim 21, wherein the ratio of 2-oxetanone to ASA is about 4: 1 or less. The method of claim 21, wherein the ratio of 2-oxetanone to ASA is about 2: 1 or less. 5. The method of claim 1, wherein the ratio of 2-oxetanone to ASA is at least about 1: 9. 6. The method of claim 24, wherein the ratio of 2-oxetanone to ASA is at least about 1: 4. The method of claim 24, wherein the ratio of 2-oxetanone to ASA is at least about 1: 2. A method of making paper under alkaline conditions, comprising providing a sizing agent comprising alkenyl succinic anhydride (ASA) and 2-oxetanone that is not solid at 35 ° C., and sizing the paper with the sizing agent. . 28. The method of claim 27 wherein the paper is internally sized with a sizing agent. A paper made by the method of claim 27 or 28. A method of using the paper of claim 29 in a high speed machining or electronic copying operation.